CN103950640A - Package and storage method of bitter almond kernel decoction piece - Google Patents

Package and storage method of bitter almond kernel decoction piece Download PDF

Info

Publication number
CN103950640A
CN103950640A CN201410213198.1A CN201410213198A CN103950640A CN 103950640 A CN103950640 A CN 103950640A CN 201410213198 A CN201410213198 A CN 201410213198A CN 103950640 A CN103950640 A CN 103950640A
Authority
CN
China
Prior art keywords
group
semen armeniacae
armeniacae amarae
materical crude
medicine materical
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201410213198.1A
Other languages
Chinese (zh)
Inventor
兰志琼
卢先明
蒋桂华
马逾英
邓晶晶
张丽娟
刘晓芬
潘晓丽
杨露
卞金辉
陈思敏
张慧慧
于宗强
郑佳
连艳
高必兴
陈虹宇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chengdu University of Traditional Chinese Medicine
Original Assignee
Chengdu University of Traditional Chinese Medicine
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Chengdu University of Traditional Chinese Medicine filed Critical Chengdu University of Traditional Chinese Medicine
Priority to CN201410213198.1A priority Critical patent/CN103950640A/en
Publication of CN103950640A publication Critical patent/CN103950640A/en
Pending legal-status Critical Current

Links

Landscapes

  • Cosmetics (AREA)

Abstract

The invention provides a package and storage method of a bitter almond kernel decoction piece. The method comprises the following steps of a, harvesting bitter almond kernel herbs, and processing and preparing the qualified bitter almond kernel decoction piece; b, adopting aluminum foils/polyethylene plastic composite films for vacuum packaging, and storing in cold places. The package and storage method of the bitter almond kernel decoction piece has the advantages that the safety, effectiveness and uniformity of the herbs can be ensured, the standard package and storage of the bitter almond kernels can be realized, and the method is convenient for popularizing and applying.

Description

A kind of packing storage practice of semen armeniacae amarae medicine materical crude slice
Technical field
The present invention relates to a kind of amygdalate packing storage practice.
Background technology
The inner wrapping prepared slices of Chinese crude drugs, also referred to as refined Chinese herbal decoction pieces, refer to processing is concocted to the qualified prepared slices of Chinese crude drugs, according to clinical common dose, with certain packing, be distributed into the inner wrapping of different size, by pharmacist, directly allocate the prepared slices of Chinese crude drugs without a kind of novel package mode weighing.The packing storage of the prepared slices of Chinese crude drugs be mainly from the viewpoint of anti-ly going mouldy, Anti-moth-eating, anti-medicine materical crude slice variable color and anti-bellding etc., traditional method mainly adopts gunnysack, thin bamboo strip basket etc., the packings such as carton, plastic bag have been there is afterwards, being sold to client takes, after scattered taking, to re-use the mode of paper bag and plastic bag packaging.In recent years, the prepared slices of Chinese crude drugs that in succession occur inner wrapping at various big hospital, pharmacy etc.But the packing of inner wrapping medicine materical crude slice are multifarious at present, there are deposited paper material in sealed polyethylene plastic, plastic sheeting, pure paper material, also have nonwoven fabrics etc., wherein take and use sealed polyethylene plastic as many.Though sealed polyethylene plastic diaphaneity is high, the proterties of being convenient to medicine materical crude slice is differentiated and quality inspection, but use for a long time plastic sheeting may have potential somatic damage, also may react with the compatibility of medicine materical crude slice composition generation chemical composition, a large amount of plastic sheetings after simultaneously clinical opening is used also can cause environmental pollution; Then three kinds of materials are opaque, when storage and adjustment, are also difficult to check that prepared slice quality changes, and have certain potential safety hazard.
Character for different Chinese medicines, the storage method of selecting is not identical yet, Jiang Chunfei (Jiang Chunfei. unlike material is on keeping the impact [J] of inner wrapping prepared slices of Chinese crude drugs safe moisture. the check of capital medicines, 2005:48~49) high pressure non-toxic polyvinyl chloride bag film, kraft paper bag, fiber woven bags, wooden case, five kinds of materials of carton are carried out to contrast experiment, finally draw other four kinds of materials relatively, high pressure non-toxic polyvinyl chloride bag film can guarantee the quality of the prepared slices of Chinese crude drugs.Lu Shandan, Ma Lifei (Lu Shandan. Ma Lifei. Tang Bailing. the Primary Study [J] that Different Package material is stored perishable Chinese medicine. Chinese medicine, 1994.10,23~24) etc. 17 (10): people is by six kinds of packing such as contrast polyethylene plastic bag, wooden case, fiber woven bags, carton, seat sheet, gunnysacks, the effect that finally filters out polyethylene plastic bag is best, and wooden case takes second place.Li Lin, Zhang Zhijie (Li Lin. Zhang Zhijie. Cai Baochang. the impact of Package upon Quality of Honey-Fried Bulbus Lilii [J]. Shanghai Univ. of Traditional Chinese Medicine's journal, 2006,64~65) etc. 20 (3): people packs sweet honey-fried BULBUS LILII medicine materical crude slice respectively with polyethylene plastic bag, vacuum complex pocket and paper plastic bag, put under different condition and store, finally show that vacuum composite packaging and paper-plastic package mould bag packing than polyethylene and more can guarantee the quality of sweet honey-fried BULBUS LILII medicine materical crude slice.Yang Juanying, Ma Jiutai (Yang Juanying. Ma Jiutai. Zheng Lingli. peppermint medicine materical crude slice different materials package stability research [J]. the Shaanxi traditional Chinese medical science, 2010,1525~1527) etc. 31 (11): people tests by peppermint medicine materical crude slice different materials package stability, draw OPP/PE composite packaging peppermint medicine materical crude slice, after storage, prepared slice quality is best.Shao Hongwei, Meng Shuhuan (Shao Hongwei. Meng Shuhuan. Psoralea corylifolia storage period effective constituent and package stability are investigated [J]. CHINA JOURNAL OF CHINESE MATERIA MEDICA, 2005,30 (14): 1127~1128) select the packing such as paper bag, plastic bag, nonwoven fabrics, investigation is with the situation of change of a collection of Psoralea corylifolia medicine materical crude slice different storage period of effective constituent, and finally it advises that large packaging and storing seals in plastic bag.Ma Jiutai, Liu Feng (Ma Jiutai. Liu Feng. Chen Yanbin etc. the research [J] of wine Radix Et Rhizoma Rhei (processed) medicine materical crude slice packing. world's traditional Chinese medicine, 2010,5 (3): 215~216) etc. people to take wine Radix Et Rhizoma Rhei (processed) medicine materical crude slice be research object, select six kinds of different packing, under different condition, test, finally draw with the rhubarb decoction pieces of OPP/PE packing best in quality.The packing of the inner wrapping prepared slices of Chinese crude drugs mainly contain in sealed polyethylene plastic, plastic sheeting and apply paper material, pure paper material and nonwoven fabrics etc. at present, in hospital, pharmacy, take sealed polyethylene plastic as many.
Semen armeniacae amarae is the dry mature seed of rosaceous plant ansu apricot Prunus armeniaca L.var.ansu Maxim., Siberia apricot Prunus sibirica L., prunus mandshuricaKoehne Prunus mandshurica (Maxim.) Koehne or apricot Prunus armeniaca L..The ripening fruits of gathering summer, removes pulp and nucleocapsid, takes out seed, dries.Get clean semen armeniacae amarae, according to 2010 editions < < Chinese pharmacopoeia > > Dan methods (appendix II D) peelings [1], dry and obtain Dan semen armeniacae amarae medicine materical crude slice.The semen armeniacae amarae beginning is loaded in < < Sheng Nong's herbal classic > >, bitter tepor, slightly poisonous, enter lung, large intestine channel, the effect such as there is sending down abnormally ascending, cough-relieving, relieving asthma, relax bowel, clinical in cough and asthma, fullness sensation in chest phlegm is many, the dry constipation of intestines, blood stasis Tianjin disease such as withered grade, for conventional Chinese medicine, as loose in Maxingshigan in consumption reach consumption in 45g, Mahuang Tang from 6g-15g not etc.Semen armeniacae amarae is rich in fatty oil, in storage and custody process because be heated or make moist very easily " bellding " (claims again " going rancid ", it is the composition such as contained volatile oil, fat, carbohydrate in medicinal material, because being heated or making moist, on its surface, occur that oily mater returns soft, stickness, darkens, send oil and lose the phenomenons such as gas), " bellding " is a kind of denaturalization phenomenon, changed the original character of medicinal material, affected its due effect
Summary of the invention
Technical scheme of the present invention has been to provide a kind of amygdalate packing storage practice.
A packing storage practice for semen armeniacae amarae medicine materical crude slice, it comprises the steps:
A, semen armeniacae amarae medicinal material is gathered after, qualified semen armeniacae amarae medicine materical crude slice is concocted in processing;
B, the vacuum packaging of employing aluminium foil/vinyon compound membrane bag, the storage of cold place.
The packing storage practice of semen armeniacae amarae medicine materical crude slice of the present invention, can guarantee that safety, validity and the homogeneity of medicinal material, the present invention have realized the normalisation of semen armeniacae amarae packing packing storage, easy to utilize.
Accompanying drawing explanation
On Fig. 1: under amarogentin reference substance HPLC collection of illustrative plates: semen armeniacae amarae medicine materical crude slice sample HPLC collection of illustrative plates
Fig. 2 amarogentin calibrated curve
Fig. 3 semen armeniacae amarae medicine materical crude slice detects peroxide value comparison for the second time, and (series 1 is the front peroxide value of storage; Series 2 is the rear 1-16 group of storage peroxide value)
Fig. 4 semen armeniacae amarae medicine materical crude slice detects amarogentin content comparison (series 1: the amarogentin content before warehouse-in for the second time; Series 2: detect for the second time amarogentin content)
The maintenance of Fig. 5 semen armeniacae amarae medicine materical crude slice detects comprehensive evaluation for the second time after 3 months
The maintenance of Fig. 6 semen armeniacae amarae medicine materical crude slice is (wherein, the series one: peroxide value before storage of peroxide value detection for the third time after 6 months; Series two: peroxide value testing result for the second time; Series three: peroxide value testing result for the third time)
Fig. 7 semen armeniacae amarae medicine materical crude slice detects amarogentin content comparison (series 1: the amarogentin content detecting before storage for the third time; Series 2: the amarogentin content detecting for the third time);
The maintenance of Fig. 8 semen armeniacae amarae medicine materical crude slice detects comprehensive evaluation for the third time after 6 months
The 4th peroxide value of Fig. 9 semen armeniacae amarae medicine materical crude slice maintenance detects (series 1: peroxide value before storage; Series 2: peroxide value testing result for the second time; Series 3: peroxide value testing result for the third time; 4: the four times peroxide value testing results of series)
Figure 10 semen armeniacae amarae medicine materical crude slice detects amarogentin content comparison (series 1: semen armeniacae amarae content detection result before warehouse-in for the 4th time; 2: the four times amarogentin content detection results of series)
The maintenance of Figure 11 semen armeniacae amarae medicine materical crude slice detected comprehensive evaluation the 4th time after 12 months
The 5th peroxide value of Figure 12 semen armeniacae amarae medicine materical crude slice maintenance detects (series 1: peroxide value before storage; Series 2: peroxide value testing result for the second time; Series 3: peroxide value testing result for the third time; 4: the four times peroxide value testing results of series; 5: the five times peroxide value testing results of series)
The 5th amarogentin content detection comparison of Figure 13 semen armeniacae amarae medicine materical crude slice (series 1: amarogentin content detection result before warehouse-in; 2: the five times amarogentin content detection results of series)
The maintenance of Figure 14 semen armeniacae amarae medicine materical crude slice detected comprehensive evaluation the 5th time after 18 months
The maintenance of Figure 15 semen armeniacae amarae medicine materical crude slice is the 6th peroxide value detection (series 1: peroxide value before storage after 24 months; Series 2: peroxide value testing result for the second time; Series 3: peroxide value testing result for the third time; 4: the four times peroxide value testing results of series; 5: the five times peroxide value testing results of series; 6: the six times peroxide value testing results of series)
The 6th amarogentin content detection comparison of Figure 16 semen armeniacae amarae medicine materical crude slice (series 1: amarogentin content detection result before storage; 2: the six times amarogentin content detection results of series)
The maintenance of Figure 17 semen armeniacae amarae medicine materical crude slice detects comprehensive evaluation the 6th time
Figure 18 semen armeniacae amarae thin layer is differentiated
The maintenance of Figure 19 semen armeniacae amarae medicine materical crude slice detects comprehensive evaluation 900 days the 7th time
The evaluation of Figure 20 semen armeniacae amarae medicine materical crude slice storage maintenance effect
The specific embodiment
Embodiment 1 semen armeniacae amarae of the present invention detects test
1 experiment material
Semen armeniacae amarae medicine materical crude slice in April, 2011 (being purchased from Chengdu new lotus prepared slices of Chinese crude drugs factory), through the first penetrating judgment of Lu of pharmaceutical college of Chengdu University of Traditional Chinese Medicine, award evaluation, the Dan semen armeniacae amarae of concocting for the dry mature seed of the rose family (Rosaceae) plant apricot Prunus armeniaca L..And therefrom select endosperm its colour changed into yellow person as bellding sample after remaining person as laboratory sample.
2.1.2 instrument and equipment
Capper (SF200-400), vacuum sealer (DZ400-2D), air-conditioning (Haier), reefer chamber (Haier), polyethylene plastic bag, ox-hide haptogen paper bag, aluminium foil/vinyon compound membrane bag.
2.1.3 semen armeniacae amarae medicine materical crude slice maintenance grouping
Three factors are chosen in this experiment: packing, temperature, oxygen.Packing and temperature are intended three levels, and two levels of aerobic anaerobic, carry out Mixed orthogonal array L 18(2*3 2) Cheng Shiwu group.The group of anaerobic is vacuumized to processing, the group encapsulation process of aerobic.Each group is placed under corresponding condition: normal temperature (10~30 ℃), storehouse is placed naturally; Shady and cool place (20 ℃ are following), air conditioning chamber; Cold place (2~10 ℃), reefer chamber simulation freezer.
Table 1 Maintenance Design
Table 2L 18(2*3 2) group situation
Note: "-" represents in actual tests not reorganization not, but need to list in table for orthogonal test design and statistic analysis result, during statistics value successively with reference to the value of numbering 3,6, No. 9 groups.
2.1.4 control group setting
The 16th group: blank group, semen armeniacae amarae medicine materical crude slice is placed in original packing bag, under normal temperature, naturally places.
3 semen armeniacae amarae medicine materical crude slice maintenances detect
Before 3.1 semen armeniacae amarae medicine materical crude slice storages, detect
3.1.1 appearance character observation
Main form of observing semen armeniacae amarae medicine materical crude slice, color and luster, smell, weight, size, soft or hard degree, oil, embrittlement, adhesion degree, and infested, mouldy situation etc.With color and luster change, the degree that mildews, have or not the phenomenon of going rancid, whether infested is index comprehensive evaluation, 0~2 minute, 0 was divided into the poorlyest, 2 are divided into full marks the best.
This product is flat heart, long 1~1.3cm, wide 0.7~1.2cm, thick 0.4~0.6cm.Surface milky or yellow-white, one end point, the blunt circle of another end, plumpness, left-right asymmetry, cotyledon 2, milky, rich oil.There is special fragrance, bitter.
3.1.2.1 reagent and instrument
Reagent: amarogentin reference substance (Rui Fensi bio tech ltd, Chengdu), methylene chloride, methyl alcohol, methenyl choloride, ethyl acetate, phosphomolybdic acid, sulfuric acid, it is pure that ethanol etc. are analysis.
Instrument: Soxhlet extraction device, round-bottomed flask, evaporating dish, cold finger, funnel, separating funnel, capillary tub, vacuum drying chamber (the gloomy reliable Instrument Ltd. that tests in Shanghai, DZG-6090 type), the thin layer plate of completing, pipet 50ml, ten thousand/electronic balance (German Sartorius BP121s), thermostat water bath (Beijing Guo Hua medical apparatus and instruments factory), conical flask, volumetric flask 5ml etc.
3.1.2.2 the preparation of need testing solution
Get this product powder (crossing No. 2 sieves of pharmacopeia) 2g, put in apparatus,Soxhlet's, add methylene chloride appropriate, add hot reflux 2 hours, discard dichloromethane solution, the dregs of a decoction volatilize, and add methyl alcohol 30ml, add hot reflux 30 minutes, let cool, and filter, and filtrate is as need testing solution.
3.1.2.3 the preparation of reference substance solution
It is appropriate that precision takes amarogentin reference substance, puts in the volumetric flask of 5ml, adds methyl alcohol and dissolve, and be settled to scale, is mixed with the reference substance solution containing amarogentin 2mg/ml.
3.1.2.4 the preparation of developping agent
Get methenyl choloride-ethyl acetate-methanol-water (15:40:22:10) 100ml, at 5~10 ℃, place 12 little layereds, take out, with separating funnel, isolate lower floor's solution, be developping agent.
3.1.2.5 point sample and colour developing
According to 2010 editions Chinese pharmacopoeia appendix VI B thin-layered chromatography, test.
3.1.3 moisture inspection
According to appendix IXH toluene method of 2010 editions Chinese pharmacopoeia, measure the moisture in semen armeniacae amarae medicine materical crude slice [1].
Get semen armeniacae amarae medicine materical crude slice powder 30g, accurately weighed, put in the round-bottomed flask of 500ml, add the content that toluene 200ml calculates moisture, as shown in table 3.
Water content detection result before table 3 semen armeniacae amarae medicine materical crude slice warehouse-in
The actual aqueous ingredients aviation value of semen armeniacae amarae medicine materical crude slice is 4.6%, within the safe aqueous ingredients 5%--13% of regulation.
3.1.4 ash content inspection
According to appendix IXK total ash determination method of 2010 editions Chinese pharmacopoeia, measure the total ash [1] of semen armeniacae amarae medicine materical crude slice.
3.1.4.1 instrument: ten thousand/electronic balance (German Sartorius BP121s), Muffle furnace (Shenyang Energy-saving electric stove factory), crucible, crucible tongs etc.
3.1.4.2 experimental technique
Get bitter benevolence medicine materical crude slice powder 3g (whole No. two sieves of pharmacopeia of crossing), put in the crucible of ignition to constant weight weighed weight (accurately to 0.01g), slowly red-hot, note avoiding burning, during to complete charing, temperature to 500~600 ℃ that raise gradually, make complete ashing and to constant weight.According to residue weight, calculate the content (%) of total ash in test sample.As shown in table 4.
Total ash testing result before table 4 semen armeniacae amarae medicine materical crude slice warehouse-in
The actual total ash aviation value of semen armeniacae amarae medicine materical crude slice is 2.518%.
3.1.5 microorganism detection
According to 2010 editions Chinese pharmacopoeia appendix X III C limit test of microbe methods, check [1], result is as table 5.
Microorganism detection result before table 5 semen armeniacae amarae medicine materical crude slice warehouse-in
Note: cfu represents " colony forming units ", i.e. CFU, and cfu/g refers to the bacterial community sum containing in every gram of sample; MPN=Most Probable Number=most probable number MPN.
According to the standard that contains the preparation of the former powder of medicinal material in oral administration in 2010 editions Chinese pharmacopoeia, check, result meets the requirements.
3.1.6 the detection of peroxide value
3.1.6.1 reagent and instrument
Normal hexane, methenyl choloride, glacial acetic acid, starch indicator solution 5g.L -1, sodium thiosulphate volumetric solution (0.01mol.L -1), saturated solution of potassium iodide, the distilled water that newly boils and let cool later, ten thousand/balance (German Sartorius BP121s), millesimal balance (Shanghai Precision Scientific Apparatus Co., Ltd, YP601N), thermostat water bath (Beijing Guo Hua medical apparatus and instruments factory), Rotary Evaporators (Yuhua Instrument Co., Ltd., Gongyi City, SHZ-D (III) type), Soxhlet extraction device, funnel, pipet, iodine flask (250mL) etc.It is pure that reagent is analysis.
3.1.6.2 experimental technique
According to oil peroxidation pH-value determination pH in 2010 editions appendix IXP of Chinese pharmacopoeia and GB GB/T5535-2005:85, operate [1,109].
3.1.6.2.1 the extraction of grease
Take semen armeniacae amarae medicine materical crude slice powder (meal) 30g, put in apparatus,Soxhlet's, add normal hexane 150mL, put in water-bath and add hot reflux 2 hours, let cool, with No. 3 sintered filter funnels, filter, filtrate is put (approximately 55 ℃) decompression and solvent recovery in water-bath and, to the greatest extent, is obtained.Fatty oil content is in Table 6.
Fatty oil content before table 6 semen armeniacae amarae medicine materical crude slice warehouse-in
3.1.6.2.2 the mensuration of peroxide value
Take the grease that quality is w, accurately weighed, put in the dry iodine flask of 250mL, add methenyl choloride-glacial acetic acid (1:1) mixed solution 30mL, make to dissolve.Precision adds new system saturated solution of potassium iodide 1mL, and close plug gently jolting half a minute, is in the dark placed 3 minutes, and thin up, with sodium thiosulphate volumetric solution (0.01mol.L -1) when being titrated to solution and being light yellow, add starch indicator solution 1mL, continue to be titrated to blue disappearance, do blank test simultaneously, according to following formula, calculate:
In formula: A, B are respectively grease and the blank volumetric solution volume consuming, mL
W is grease weight, g
Result is as shown in table 7.
Peroxide value testing result before table 7 semen armeniacae amarae medicine materical crude slice warehouse-in
The peroxide value of semen armeniacae amarae medicine materical crude slice, lower than 0.11 of 2010 editions Chinese pharmacopoeia regulations, proves that the front semen armeniacae amarae prepared slice quality of warehouse-in is better.
3.1.7 the mensuration of amarogentin content
According to 2010 editions Chinese pharmacopoeia methods, carry out.
3.1.7.1 instrument and reagent
U.S. Agilent1100 high performance liquid chromatograph and auxiliary work station thereof, DAD detector, vacuum drying chamber (reliable Instrument Ltd. that tests of upper Mason, DZG-6090 type), 100000/electronic balance (German Sartorius BP211D), electronic balance (Shang Mei exact science Instrument Ltd., YP601N), ten thousand/balance (German Sartorius BP121s), BUG25-12 supersonic wave cleaning machine (Shanghai Bi Nengxin company), chromatographic column is Hypersil ODS C 18(250mm * 4.6mm, 5 μ m, Dalian Yilite Analytical Instrument Co., Ltd), acetonitrile is chromatographically pure (U.S. Fisher company), water is ultra-pure water (Milipore preparation), 0.45 μ m pin type miillpore filter.It is pure that other reagent is analysis.Amarogentin reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number 110820-200403, for assay).
3.1.7.2 chromatographic condition
Mobile phase is acetonitrile-0.1% phosphoric acid solution (8:92); Detection wavelength is 207nm.Number of theoretical plate calculates and should be not less than 7000 by amarogentin peak.Chromatographic column is Hypersil ODS C 18(250mm * 4.6mm, 5 μ m).
3.1.7.3 the preparation of reference substance solution
It is appropriate that precision takes amarogentin reference substance, puts in the volumetric flask of 10ml, adds methyl alcohol and dissolve, and be settled to scale, is mixed with every 1ml containing the solution of amarogentin 500 μ g, obtains.Fig. 1 is shown in by amarogentin reference substance HPLC collection of illustrative plates.
3.1.7.4 the preparation of need testing solution
Get the about 0.25g of this product powder (crossing sieve No. two), accurately weighed, to put in tool plug conical flask, precision adds methyl alcohol 25ml, close plug, weighed weight, ultrasonic processing (power 250W, frequency 50kHz) 30 minutes, let cool, more weighed weight, with methyl alcohol, supply the weight of less loss, shake up, filter, precision measures subsequent filtrate 5ml, put in 50ml measuring bottle, add 50% methyl alcohol and be diluted to scale, shake up, filter, get continuous filter and tuck in, obtain.
3.1.7.5 the drafting of calibrated curve
The accurate reference substance solution sample introduction of drawing 2ul, 6ul, 10ul, 12ul, 16ul, 20ul, the volume of reference substance solution sample size of take is abscissa X, chromatographic peak area is that ordinate Y carries out linear regression, the results are shown in Figure 2.
Amarogentin is good in 0.8ug~8ug scope internal linear relation, and regression equation is: y=479.85x+291.93 (R 2=0.9999).
3.1.7.6 precision test
The accurate reference substance solution 10ul that draws, continuous sample introduction 5 times, measures amarogentin peak area, the results are shown in Table 8.
Table 8 amarogentin Precision Experiment result
RSD is 0.373%, shows that the degree of precision of instrument is good.
3.1.7.7 duplicability test
Get same sample, by parallel 5 parts of the need testing solutions of producing of method under " 7.4 " item, measure respectively, calculate amarogentin content, the results are shown in Table 9.
Table 9 amarogentin duplicability experimental result
RSD is 0.87%, shows that this condition duplicability is good.
3.1.7.8 stability test
By need testing solution in room temperature, place 0,2,4,8,12, sample introduction 10ul measures respectively after 24h, measures amarogentin peak area, the results are shown in Table 10.
Table 10 amarogentin stability experiment result
RSD is 0.56%, shows that need testing solution is at room temperature placed in 24h basicly stable under this experiment condition.
3.1.7.9 recovery test
Get 9 parts, semen armeniacae amarae medicine materical crude slice powder, each about 0.1300g, accurately weighed.By 80%, 100%, 120% precision of its content, add amarogentin reference substance appropriate respectively, according to " 7.4 " bar method, prepare need testing solution and measure content, calculate average recovery, according to operating under assay item, knot is stayed in Table 11.
The determination of recovery rates result of table 11 amarogentin
Average recovery rate is 100.1%, RSD=2.49%, shows that this law percent recovery is better.
3.1.7.10 the mensuration of sample
Get semen armeniacae amarae medicine materical crude slice and make need testing solution by " 3.1.7.4 ", measure, with external standard method, calculate the content of amarogentin.As shown in table 12.
The measurement result of amarogentin before table 12 semen armeniacae amarae medicine materical crude slice warehouse-in
Semen armeniacae amarae medicine materical crude slice sample amarogentin content is higher, proves that the front semen armeniacae amarae prepared slice quality of warehouse-in is better.
3.2 semen armeniacae amarae medicine materical crude slice storages detect after 3 months for the second time
3.2.1 appearance character observation
Main form of observing medicinal material, color and luster, smell, weight, size, soft or hard degree, oil, embrittlement, adhesion degree, and infested, mouldy situation etc.
3.2.1.1 proterties comprehensive evaluation
With semen armeniacae amarae medicine materical crude slice color and luster change, cracked degree, have or not the phenomenon of going rancid, whether infested is index, comprehensive evaluation.
As shown in table 13.
Table 13 semen armeniacae amarae medicine materical crude slice detects ocular estimate for the second time
From table 13, preserve after 3 months, each group is full marks, illustrate semen armeniacae amarae medicine materical crude slice put in storage storage after 3 months in order, in the summer that at once will step into high temperature, check storehouse, keep clean and dry.
3.2.1.2 infested degree
Grab sample, totally 10 groups, get semen armeniacae amarae medicine materical crude slice 50g for every group, observe to calculate a semen armeniacae amarae medicine materical crude slice number that wherein has insect bite vestige, with/50gWei unit evaluates the infested degree of medicinal material.All do not find infested semen armeniacae amarae medicine materical crude slice, the storage effect to the 90 days of each group is all very good, is about to step into season in midsummer, note the clean and humidity of storehouse.
3.2.2 moisture inspection
By appendix IX H toluene method of version Chinese pharmacopoeia in 2010, measure semen armeniacae amarae medicine materical crude slice moisture.Get semen armeniacae amarae medicine materical crude slice powder 40g, accurately weighed, put in the round-bottomed flask of 500ml, add the content that toluene 200ml calculates moisture, as shown in table 14.
The maintenance of table 14 semen armeniacae amarae medicine materical crude slice detects aqueous ingredients (%) for the second time
When the maintenance of semen armeniacae amarae medicine materical crude slice detects after 3 months for the second time, moisture content change is little, in safe aqueous ingredients 13.0%.
3.2.3 peroxide value inspection
The peroxide value that detects semen armeniacae amarae medicine materical crude slice with reference to test method under 3.1.6.2.2 item, the results are shown in Table 15.
Table 15 maintenance for the second time detects semen armeniacae amarae medicine materical crude slice peroxide value testing result
The maintenance of semen armeniacae amarae medicine materical crude slice detects for the second time 0.005076 before peroxide value and warehouse-in and compares each group and all have increasing in various degree after 3 months, but the peak 0.11 of all stipulating lower than pharmacopeia, showing to preserve semen armeniacae amarae medicine materical crude slice after 3 months has had slight denaturalization phenomenon to occur, but still meets medicinal standard.
As shown in Figure 3.Wherein the 7th group (ox-hide haptogen paper, sealing, normal temperature), the 4th group of (polyethylene plastic bag, sealing, normal temperature), the 5th group of (polyethylene plastic bag, sealing, shady and cool), the rising amplitude of the 6th group of (polyethylene plastic bag, sealing, refrigeration) peroxide value is maximum; The 9th group (ox-hide haptogen paper, sealing, refrigeration), the 11 group of (aluminium foil/vinyon compound membrane bag, vacuum, cool place), the 12 group of (aluminium foil/vinyon compound membrane bag, vacuum, refrigeration), the 15 group of (aluminium foil/vinyon compound membrane bag, sealing, refrigeration), the 16 group of (control group) peroxide value changes minimum.
3.2.4 amarogentin assay
The amarogentin content that detects semen armeniacae amarae medicine materical crude slice with reference to test method under 3.1.7.10 item, the results are shown in Table 16.
Table 16 maintenance for the second time detects semen armeniacae amarae medicine materical crude slice amarogentin content detection result
When maintenance detects after 3 months for the second time, each is organized semen armeniacae amarae medicine materical crude slice and surveys amarogentin content and front 2.69% compare with warehouse-in, all has reduction, and showing to preserve semen armeniacae amarae medicine materical crude slice after 3 months has had denaturalization phenomenon, sees Fig. 4.
Control group wherein, the 9th group (ox-hide haptogen paper bag, sealing, refrigeration) changes minimum.Other each group all reduces more.
3.2.5 Analysis of test results
The storage of semen armeniacae amarae medicine materical crude slice warehouse-in is after 3 months, carry out the detection for the second time of semen armeniacae amarae medicine materical crude slice maintenance test, in test, pass through to detect semen armeniacae amarae medicine materical crude slice moisture, peroxide value, amarogentin content and appearance character comprehensive evaluation, substitution formula: comprehensive evaluation index=A i/ 2*0.1+0.013071/B i* 0.4+C i* 0.5
(A iocular estimate; B iperoxide value; C iamarogentin content)
Score value is higher shows that semen armeniacae amarae medicine materical crude slice storage effect is better, as shown in Figure 5.
Before showing respectively to organize semen armeniacae amarae prepared slice quality and putting in storage, all decline to some extent, wherein the 7th group (ox-hide haptogen paper bag packing, sealing, room temperature storage) mass change is minimum, and storage effect is best; The 11 group of (aluminium foil/vinyon compound membrane bag packing, vacuum, cool place) storage effect is the poorest.
Maintenance effect is followed successively by the 11 group of first group of > of the tenth group of > of the 6th group of > of the 7th group of > of maintenance the 4th group of > of the 8th group of > of the 5th group of > blank group > second group of > the 12 group of > the 15 group of > of the 13 group of > of the 3rd group of > of the 14 group of > of the 9th group of >.
3.3 semen armeniacae amarae medicine materical crude slice storages detect after 6 months for the third time
3.3.1 appearance character observation
Main form of observing medicinal material, color and luster, smell, weight, size, soft or hard degree, oil, embrittlement, adhesion degree, and infested, mouldy situation etc.With semen armeniacae amarae medicine materical crude slice color and luster change, cracked degree, have or not the phenomenon of going rancid, whether infested is index, comprehensive evaluation.Shown in table 17.
Table 17 semen armeniacae amarae medicine materical crude slice detects ocular estimate for the third time
From table 17, preserving while detecting for the third time after 6 months compares when semen armeniacae amarae medicine materical crude slice presentation quality detects after 3 months for the second time with storage change very little.
3.3.2 moisture inspection
By appendix IX H toluene method of version Chinese pharmacopoeia in 2010, measure semen armeniacae amarae medicine materical crude slice moisture.Get semen armeniacae amarae medicine materical crude slice powder 40g, accurately weighed, put in the round-bottomed flask of 500ml, add the content that toluene 200ml calculates moisture.Shown in table 18.
The maintenance of table 18 semen armeniacae amarae medicine materical crude slice detects aqueous ingredients (%) for the third time
When the maintenance of semen armeniacae amarae medicine materical crude slice detects after 6 months for the third time, moisture still changes not quite, at safe aqueous ingredients below 13.0%.
3.3.3 peroxide value inspection
The peroxide value that detects semen armeniacae amarae medicine materical crude slice with reference to test method under 3.1.6.2.2 item, the results are shown in Table 19.
Table 19 maintenance for the third time detects semen armeniacae amarae medicine materical crude slice peroxide value testing result
When maintenance detects after 6 months for the third time, each is organized semen armeniacae amarae peroxide value that medicine materical crude slice is surveyed and compares with the peroxide value 0.005076 that semen armeniacae amarae medicine materical crude slice before warehouse-in detects, and reduces slowly, shows the storage of semen armeniacae amarae medicine materical crude slice in order.
As shown in Figure 6.The result that peroxide value detects is for the third time all low than the peroxide value before warehouse-in.The highest is the 16 group (being control group), and it is all not obvious that other respectively organizes current difference.
3.3.4 amarogentin assay
The amarogentin content that detects semen armeniacae amarae medicine materical crude slice with reference to test method under 3.1.7.10 item, the results are shown in Table 20.
Table 20 maintenance for the third time detects semen armeniacae amarae medicine materical crude slice amarogentin content detection result
When maintenance detects after 6 months for the third time, each is organized semen armeniacae amarae medicine materical crude slice and surveys amarogentin content and front 2.69% compare with warehouse-in, all has reduction, and showing to preserve semen armeniacae amarae medicine materical crude slice after 6 months has had denaturalization phenomenon.See Fig. 7
Control group wherein, the 9th group of (ox-hide haptogen paper bag, sealing, refrigeration) group changes minimum.Other each group all reduces more.
3.3.5 Analysis of test results
The storage of semen armeniacae amarae medicine materical crude slice warehouse-in, after 6 months, is carried out the detection for the third time of semen armeniacae amarae medicine materical crude slice maintenance test, passes through to detect semen armeniacae amarae medicine materical crude slice peroxide value, amarogentin content and appearance character comprehensive evaluation, substitution formula in test:
Comprehensive evaluation index=A i/ 2*0.1+0.004606/B i* 0.4+C i* 0.5
(A iocular estimate; B iperoxide value; C iamarogentin content)
Score value is higher shows that semen armeniacae amarae medicine materical crude slice storage effect is better, as shown in Figure 8.
Test shows respectively to organize before semen armeniacae amarae prepared slice quality is put in storage all decline, and wherein the tenth group (aluminium foil/vinyon compound membrane bag packing, vacuum, room temperature storage) mass change is minimum, and storage effect is best; The 13 group of (aluminium foil/vinyon compound membrane bag packing, sealing, normal temperature) storage effect is the poorest.
Maintenance effect is followed successively by the 13 group of the 15 group of > of the tenth group of > of maintenance second group of > the 4th group of > of first group of > of the 11 group of > of the 5th group of > the 9th group of > the 8th group of > of the 6th group of > blank group > the 7th group of > the 12 group of > the 14 group of > of the 3rd group of >
3.4 semen armeniacae amarae medicine materical crude slice storages detected for the 4th time after 12 months
3.4.1 appearance character observation
Main form of observing medicinal material, color and luster, smell, weight, size, soft or hard degree, oil, embrittlement, adhesion degree, and infested, mouldy situation etc.With semen armeniacae amarae medicine materical crude slice color and luster change, cracked degree, have or not the phenomenon of going rancid, whether infested is index, comprehensive evaluation.Shown in table 21.
Table 21 semen armeniacae amarae medicine materical crude slice detects ocular estimate the 4th time
From table 21, preserve after 12 months while detecting for the 4th time the variation of comparing when semen armeniacae amarae medicine materical crude slice presentation quality detects after 6 months for the third time with storage very little.But there is the brown medicine materical crude slice of minority to occur.
3.4.2 moisture inspection
By appendix IX H toluene method of version Chinese pharmacopoeia in 2010, measure semen armeniacae amarae medicine materical crude slice moisture.Get semen armeniacae amarae medicine materical crude slice powder 40g, accurately weighed, put in the round-bottomed flask of 500ml, add the content that toluene 200ml calculates moisture.Shown in table 22.
The maintenance of table 22 semen armeniacae amarae medicine materical crude slice detects aqueous ingredients (%) the 4th time
When the maintenance of semen armeniacae amarae medicine materical crude slice detected for the 4th time after 12 months, moisture still changes not quite, at safe aqueous ingredients below 13.0%.3.4.3 peroxide value inspection
The peroxide value that detects semen armeniacae amarae medicine materical crude slice with reference to test method under 3.1.6.2.2 item, the results are shown in Table 23.
The 4th maintenance of table 23 detects semen armeniacae amarae medicine materical crude slice peroxide value testing result
When maintenance detected for the 4th time after 12 months, each is organized semen armeniacae amarae peroxide value that medicine materical crude slice is surveyed and compares with peroxide value 0.005076 of the front semen armeniacae amarae medicine materical crude slice detection of warehouse-in, have rising, has reduction, but all in the specialized range of pharmacopeia, meets medicinal standard.
As shown in Figure 9.The result of the 4th peroxide value detection is all high than the peroxide value detecting for the second time.The 14 group of (aluminium foil/vinyon compound membrane bag, sealing, cool place), the 15 group of (aluminium foil/vinyon compound membrane bag, sealing, refrigeration), the 9th group of (ox-hide haptogen paper, sealing, refrigeration), the peroxide value of the 11 group of (aluminium foil/vinyon compound membrane bag, vacuum, cool place) group is larger; Second group (polyethylene plastic bag, vacuum, cool place), the 3rd group (polyethylene plastic bag, vacuum, refrigeration), the 6th group (polyethylene plastic bag, sealing, refrigeration), the 7th group of (ox-hide haptogen paper bag, sealing, normal temperature), the 8th group of (ox-hide haptogen paper bag, sealing, cool place) group peroxide value all than warehouse-in before peroxide value little.
3.4.4 amarogentin assay
The amarogentin content that detects semen armeniacae amarae medicine materical crude slice with reference to test method under 3.1.7.10 item, the results are shown in Table 24.
The 4th maintenance of table 24 detects semen armeniacae amarae medicine materical crude slice amarogentin content detection result
When maintenance detected for the 4th time after 12 months, each is organized semen armeniacae amarae medicine materical crude slice and surveys amarogentin content and put front 2.69% in storage and compare, and all has reduction, and showing to preserve semen armeniacae amarae medicine materical crude slice after 12 months has had denaturalization phenomenon, sees Figure 10.
Wherein the 9th group (ox-hide haptogen paper bag, sealing, refrigeration), the 15 group (aluminium foil/vinyon compound membrane bag, sealing, refrigeration) changes minimum.Other each group all reduces more.
3.4.5 Analysis of test results
The storage of semen armeniacae amarae medicine materical crude slice warehouse-in, after 12 months, detects for the 4th time that carries out semen armeniacae amarae medicine materical crude slice maintenance test, passes through to detect semen armeniacae amarae medicine materical crude slice peroxide value, amarogentin content and appearance character comprehensive evaluation, substitution formula in test:
Comprehensive evaluation index=A i/ 2*0.1+0.009212/B i* 0.4+C i* 0.5
(A iocular estimate; B iperoxide value; C iamarogentin content)
Score value is higher shows that semen armeniacae amarae medicine materical crude slice storage effect is better, as shown in figure 11.
Test shows respectively to organize before semen armeniacae amarae prepared slice quality is put in storage all decline, and wherein the 3rd group (polyethylene plastic bag packing, vacuum, chilled storage) mass change is minimum, and storage effect is best; The 14 group of (aluminium foil/vinyon compound membrane bag, sealing, cool place) storage effect is the poorest.Blank group is than other group inequality.
Maintenance effect is followed successively by the 14 group of > blank group of the 9th group of > of first group of > of the 8th group of > of the 7th group of > of the 6th group of > of second group of > of the 3rd group of > of maintenance the tenth group of > the 12 group of > the 4th group of > of the 11 group of > of the 15 group of > of the 13 group of > of the 5th group of >
3.5 semen armeniacae amarae medicine materical crude slice storages detected for the 5th time after 18 months
3.5.1 appearance character observation
Main form of observing medicinal material, color and luster, smell, weight, size, soft or hard degree, oil, embrittlement, adhesion degree, and infested, mouldy situation etc.With semen armeniacae amarae medicine materical crude slice color and luster change, cracked degree, have or not the phenomenon of going rancid, whether infested is index, comprehensive evaluation.As shown in Table 25.
Table 25 semen armeniacae amarae medicine materical crude slice detects ocular estimate the 5th time
From table 24, preserve after 18 months while detecting for the 5th time the variation of comparing when semen armeniacae amarae medicine materical crude slice presentation quality detects for the 4th time after 12 months with storage more obvious.In the packing of every type, the color and luster of almond and the temperature of storage present obvious incidence relation, aerobic and anaerobic, and the semen armeniacae amarae medicine materical crude slice color of preserving under shady and cool environment is shallower than the semen armeniacae amarae medicine materical crude slice color of preserving under normal temperature and is deeper than the semen armeniacae amarae medicine materical crude slice of preserving under cold place.
3.5.2 moisture inspection
By appendix IX H toluene method of version Chinese pharmacopoeia in 2010, measure semen armeniacae amarae medicine materical crude slice moisture.Get semen armeniacae amarae medicine materical crude slice powder 40g, accurately weighed, put in the round-bottomed flask of 500ml, add the content that toluene 200ml calculates moisture.Shown in table 26.
The maintenance of table 26 semen armeniacae amarae medicine materical crude slice detects aqueous ingredients (%) the 5th time
When the maintenance of semen armeniacae amarae medicine materical crude slice detected for the 5th time after 18 months, moisture still changes not quite, at safe aqueous ingredients below 13.0%.
3.5.3 peroxide value inspection
The peroxide value that detects semen armeniacae amarae medicine materical crude slice with reference to test method under 3.1.6.2.2 item, the results are shown in Table 27.
The 5th maintenance of table 27 detects semen armeniacae amarae medicine materical crude slice peroxide value testing result
When maintenance detected for the 5th time after 18 months, each is organized semen armeniacae amarae peroxide value that medicine materical crude slice is surveyed and compares with peroxide value 0.005076 of the front semen armeniacae amarae medicine materical crude slice detection of warehouse-in, have rising, has reduction, but all in the specialized range of pharmacopeia, meets medicinal standard.
As shown in figure 12.The result of the 5th peroxide value detection is all high than the peroxide value detecting for the second time.Control group, the 4th group of (polyethylene plastic bag, sealing, normal temperature), the 14 group (aluminium foil/vinyon compound membrane bag, sealing, cool place), the 12 group of (aluminium foil/vinyon compound membrane bag, vacuum, cool place), second group of (polyethylene plastic bag, vacuum, cool place) peroxide value of group is larger; The tenth group (aluminium foil/vinyon compound membrane bag, vacuum, normal temperature); The peroxide value of first group of (polyethylene plastic bag, vacuum, normal temperature) group is all little than the peroxide value before warehouse-in.
3.5.4 amarogentin assay
The amarogentin content that detects semen armeniacae amarae medicine materical crude slice with reference to test method under 3.1.7.10 item, the results are shown in Table 28, Figure 13.
The 5th maintenance of table 28 detects semen armeniacae amarae medicine materical crude slice amarogentin content detection result
When maintenance detected for the 5th time after 18 months, each is organized semen armeniacae amarae medicine materical crude slice and surveys amarogentin content and put front 2.69% in storage and compare, and all has reduction, and showing to preserve semen armeniacae amarae medicine materical crude slice after 18 months has had denaturalization phenomenon.
Wherein the 15 group (aluminium foil/vinyon compound membrane bag, sealing, refrigeration), the 6th group (polyethylene plastic bag, sealing, refrigeration) changes minimum.Other each group all reduces more.
3.5.5 Analysis of test results
The storage of semen armeniacae amarae medicine materical crude slice warehouse-in, after 18 months, detects for the 5th time that carries out semen armeniacae amarae medicine materical crude slice maintenance test, passes through to detect semen armeniacae amarae medicine materical crude slice peroxide value, amarogentin content and appearance character comprehensive evaluation, substitution formula in test:
Comprehensive evaluation index=A i/ 2*0.1+0.005401/B i* 0.4+C i* 0.5
(A iocular estimate; B iperoxide value; C iamarogentin content)
Score value is higher shows that semen armeniacae amarae medicine materical crude slice storage effect is better, as shown in figure 14.
Test shows respectively to organize before semen armeniacae amarae prepared slice quality is put in storage all decline, and wherein the tenth group (aluminium foil/vinyon compound membrane bag packing, vacuum, room temperature storage) mass change is minimum, and storage effect is best; The 4th group of (polyethylene plastic bag packing, sealing, normal temperature) storage effect is the poorest.Blank group compared with the 4th group outward than other group inequality.
Maintenance effect is followed successively by the 4th group of second group of > blank group > of the 3rd group of > the 8th group of > of the 11 group of > of first group of > of the 13 group of > the 5th group of > the 12 group of > of the 14 group of > of the 7th group of > of the 6th group of > of maintenance the 9th group of > of the 15 group of > of the tenth group of >
3.6 semen armeniacae amarae medicine materical crude slice storages detected for the 6th time after 24 months
3.6.1 appearance character observation
Main form of observing medicinal material, color and luster, smell, weight, size, soft or hard degree, oil, embrittlement, adhesion degree, and infested, mouldy situation etc.With semen armeniacae amarae medicine materical crude slice color and luster change, cracked degree, have or not the phenomenon of going rancid, whether infested is index, comprehensive evaluation.Shown in table 29.
Table 29 semen armeniacae amarae medicine materical crude slice detects ocular estimate the 6th time
From table 29, preserve after 24 months while detecting for the 6th time the variation of comparing when semen armeniacae amarae medicine materical crude slice presentation quality detects for the 5th time after 18 months with storage more obvious.In the packing of every type, the color and luster of almond and the temperature of storage present obvious incidence relation, no matter be under aerobic conditions or under oxygen free condition, the semen armeniacae amarae medicine materical crude slice color of preserving under shady and cool environment is shallower than the semen armeniacae amarae medicine materical crude slice color of preserving under normal temperature but is deeper than the semen armeniacae amarae medicine materical crude slice of preserving under cold storage environment.
3.6.2 moisture inspection
By appendix IX H toluene method of version Chinese pharmacopoeia in 2010, measure semen armeniacae amarae medicine materical crude slice moisture.Get semen armeniacae amarae medicine materical crude slice powder 40g, accurately weighed, put in the round-bottomed flask of 500ml, add the content that toluene 200ml calculates moisture.Shown in table 30.
The maintenance of table 30 semen armeniacae amarae medicine materical crude slice detects aqueous ingredients (%) the 6th time
When the maintenance of semen armeniacae amarae medicine materical crude slice detected for the 6th time after 24 months, moisture still changes not quite, at safe aqueous ingredients below 13.0%.
3.6.3 peroxide value inspection
The peroxide value that detects semen armeniacae amarae medicine materical crude slice with reference to test method under 3.1.6.2.2 item, the results are shown in Table 31.
The 6th maintenance of table 31 detects semen armeniacae amarae medicine materical crude slice peroxide value testing result
When maintenance detected for the 6th time after 24 months, each is organized semen armeniacae amarae peroxide value that medicine materical crude slice is surveyed and compares with peroxide value 0.005076 of the front semen armeniacae amarae medicine materical crude slice detection of warehouse-in, have rising, also has reduction, but all in the specialized range of pharmacopeia, meets medicinal standard.
3.6.4 amarogentin assay
The amarogentin content that detects semen armeniacae amarae medicine materical crude slice with reference to test method under 3.1.7.10 item, the results are shown in Table 32.
The 6th maintenance of table 32 detects semen armeniacae amarae medicine materical crude slice amarogentin content detection result
When maintenance detected for the 6th time after 24 months, each is organized semen armeniacae amarae medicine materical crude slice and surveys amarogentin content and put front 2.69% in storage and compare, and all has reduction, and showing to preserve semen armeniacae amarae medicine materical crude slice after 24 months has had denaturalization phenomenon, sees Figure 16.
Wherein the 9th group (ox-hide haptogen paper bag, sealing, refrigeration), the 3rd group (polyethylene plastic bag, vacuum, refrigeration) changes minimum.Other each group all reduces more.
3.6.5 Analysis of test results
The storage of semen armeniacae amarae medicine materical crude slice warehouse-in, after 24 months, detects for the 6th time that carries out semen armeniacae amarae medicine materical crude slice maintenance test, passes through to detect semen armeniacae amarae medicine materical crude slice peroxide value, amarogentin content and appearance character comprehensive evaluation, substitution formula in test:
Comprehensive evaluation index=A i/ 2*0.1+0.005401/B i* 0.4+C i* 0.5
(A iocular estimate; B iperoxide value; C iamarogentin content)
Score value is higher shows that semen armeniacae amarae medicine materical crude slice storage effect is better, as shown in figure 17.
Test shows respectively to organize before semen armeniacae amarae prepared slice quality is put in storage all decline, and wherein the 3rd group (polyethylene plastic bag packing, vacuum, chilled storage) mass change is minimum, and storage effect is best; The 5th group of (polyethylene plastic bag packing, sealing, cool place) storage effect is the poorest.Blank group storage effect is placed in the middle.
Maintenance effect is followed successively by the 5th group of the 8th group of > of the 12 group of > blank group > the 14 group of > the 13 group of > first group of > of the 7th group of > of the 4th group of > of the 11 group of > of the 6th group of > of the tenth group of > of the 3rd group of > of maintenance second group of > of the 15 group of > of the 9th group of >
3.7 semen armeniacae amarae medicine materical crude slice packing storages detect for 900 days the 7th time
3.7.1 appearance character observation
Main form of observing medicinal material, color and luster, smell, weight, size, soft or hard degree, oil, embrittlement, adhesion degree, and infested, mouldy situation etc.Comprehensive evaluation.Shown in table 33.
Table 33 semen armeniacae amarae medicine materical crude slice detects ocular estimate the 7th time
Group Color and luster Mildew Go rancid Infested Comprehensive evaluation
First group Brown color Nothing Nothing Nothing 1.6
Second group Ivory buff Nothing Nothing Nothing 1.85
The 3rd group Yellow-white Nothing Nothing Nothing 1.85
The 4th group Brown color Nothing Nothing Nothing 1.65
The 5th group Yellow-white Nothing Nothing Nothing 1.85
The 6th group Yellow-white Nothing Nothing Nothing 1.85
The 7th group Brown color Slightly Nothing Nothing 1.6
The 8th group Yellow-white Slightly Nothing Nothing 1.65
The 9th group Yellow-white Nothing Nothing Nothing 1.8
The tenth group Sundown Nothing Nothing Nothing 1.75
The 11 group Yellow-white Nothing Nothing Nothing 1.85
The 12 group Yellow-white Nothing Nothing Nothing 1.85
The 13 group Sundown Nothing Nothing Nothing 1.7
The 14 group Yellow-white Nothing Nothing Nothing 1.85
The 15 group Yellow-white Nothing Nothing Nothing 1.85
Blank group Brown color Nothing Nothing Nothing 1.6
From table 33, when while preserving 900 days the 7th time detection, semen armeniacae amarae medicine materical crude slice presentation quality detects for 700 days the 6th time with storage, comparing, it is more obvious to change.In the packing of every type, the color and luster of almond and the temperature of storage present obvious incidence relation, no matter be under aerobic conditions or under oxygen free condition, the semen armeniacae amarae medicine materical crude slice color of preserving under shady and cool environment is shallower than the semen armeniacae amarae medicine materical crude slice color of preserving under normal temperature but is deeper than the semen armeniacae amarae medicine materical crude slice of preserving under cold storage environment.
3.7.2 thin layer is differentiated
According to thin-layered chromatography (appendix VI B) test, result is as Figure 18.
3.7.3 moisture inspection
By appendix IXH toluene method of version Chinese pharmacopoeia in 2010, measure semen armeniacae amarae medicine materical crude slice moisture.The results are shown in Table 34.
The maintenance of table 34 semen armeniacae amarae medicine materical crude slice detects aqueous ingredients (%) the 6th time
Group 1 2 3 Aviation value
First group 4.48 4.88 4.72 4.69
Second group 4.16 4.56 4.48 4.40
The 3rd group 4.84 4.44 4.88 4.72
The 4th group 4.84 4.84 5.20 4.96
The 5th group 4.88 5.00 5.28 5.05
The 6th group 4.60 4.80 4.48 4.63
The 7th group 4.68 5.20 4.68 4.85
The 8th group 4.20 4.32 4.60 4.37
The 9th group 5.64 5.80 5.24 5.56
The tenth group 4.36 4.48 4.56 4.47
The 11 group 5.20 5.12 4.92 5.08
The 12 group 4.96 5.00 5.20 5.05
The 13 group 4.64 4.76 4.84 4.75
The 14 group 4.72 4.92 5.12 4.92
The 15 group 4.36 4.76 4.40 4.51
Blank group 5.28 5.40 4.76 5.15
When semen armeniacae amarae medicine materical crude slice maintenance 900 days the 7th time detects, moisture still changes not quite, at safe aqueous ingredients below 13%.
3.7.4 ash content inspection
By 2010 editions Chinese pharmacopoeia appendix IX K total ash determination methods, measure the total ash of semen armeniacae amarae medicine materical crude slice.The results are shown in Table 35.
Total ash testing result before table 35 semen armeniacae amarae medicine materical crude slice warehouse-in
Group 1 2 3 Aviation value (%)
First group 2.459 2.497 2.504 2.487
Second group 2.430 2.515 2.464 2.470
The 3rd group 2.410 2.547 2.482 2.480
The 4th group 2.452 2.444 2.520 2.472
The 5th group 2.521 2.482 2.500 2.501
The 6th group 2.446 2.495 2.487 2.476
The 7th group 2.499 2.426 2.458 2.461
The 8th group 2.494 2.508 2.514 2.505
The 9th group 2.503 2.468 2.484 2.485
The tenth group 2.472 2.496 2.493 2.487
The 11 group 2.464 2.508 2.464 2.479
The 12 group 2.465 2.512 2.415 2.464
The 13 group 2.447 2.459 2.435 2.447
The 14 group 2.431 2.483 2.472 2.462
The 15 group 2.461 2.497 2.509 2.489
Blank group 2.430 2.495 2.549 2.491
3.7.5 microorganism detection
According to 2010 editions Chinese pharmacopoeia appendix X III C limit test of microbe methods, check, the results are shown in Table 36.
900 days microorganism detection results of table 36 semen armeniacae amarae medicine materical crude slice warehouse-in
Note: cfu represents " colony forming units ", i.e. CFU, and cfu/g refers to the bacterial community sum containing in every gram of sample.
3.7.6 peroxide value inspection
The peroxide value that detects semen armeniacae amarae medicine materical crude slice with reference to test method under 2.1.6.2.2 item, records and the results are shown in Table 37.
The 7th maintenance of table 37 detects semen armeniacae amarae medicine materical crude slice peroxide value testing result
Group 1 2 3 Aviation value
First group 0.005839 0.006037 0.006586 0.006154
Second group 0.005016 0.004940 0.004391 0.004782
The 3rd group 0.003579 0.003842 0.004391 0.003937
The 4th group 0.005290 0.005488 0.006037 0.005605
The 5th group 0.004963 0.004940 0.004940 0.004948
The 6th group 0.004379 0.003842 0.003842 0.004021
The 7th group 0.006131 0.006037 0.006037 0.006068
The 8th group 0.006492 0.006037 0.005488 0.006006
The 9th group 0.004773 0.003842 0.004391 0.004335
The tenth group 0.005290 0.004391 0.004940 0.004874
The 11 group 0.005255 0.004940 0.004391 0.004862
The 12 group 0.004671 0.004391 0.003842 0.004301
The 13 group 0.006423 0.005488 0.005488 0.005800
The 14 group 0.005311 0.004940 0.004940 0.005064
The 15 group 0.004176 0.003842 0.003842 0.003953
Blank group 0.006985 0.005488 0.006037 0.006170
When maintenance detected for the 7th time after 900 days, each is organized semen armeniacae amarae peroxide value that medicine materical crude slice is surveyed and compares with peroxide value 0.005076 of the front semen armeniacae amarae medicine materical crude slice detection of warehouse-in, have rising, also has reduction, but all in the specialized range of pharmacopeia, meets medicinal standard.
3.7.7 amarogentin assay
The amarogentin content that detects semen armeniacae amarae medicine materical crude slice with reference to test method under 2.1.7.10 item, records and the results are shown in Table 38.
The 7th maintenance of table 38 detects semen armeniacae amarae medicine materical crude slice amarogentin content detection result
Group 1 2 3 Aviation value
First group 2.026 1.994 1.990 2.003
Second group 2.167 2.080 2.103 2.117
The 3rd group 2.238 2.172 2.212 2.207
The 4th group 1.945 2.024 2.011 1.993
The 5th group 2.042 2.035 2.045 2.041
The 6th group 2.077 2.165 2.231 2.158
The 7th group 2.057 2.121 2.078 2.085
The 8th group 2.112 2.100 2.104 2.105
The 9th group 2.278 2.453 2.356 2.362
The tenth group 2.195 2.139 2.065 2.133
The 11 group 2.060 2.197 2.088 2.115
The 12 group 2.291 2.190 2.220 2.234
The 13 group 2.020 2.072 2.054 2.049
The 14 group 2.081 2.202 2.182 2.155
The 15 group 2.134 2.251 2.344 2.243
Blank group 1.911 2.011 1.993 1.972
When maintenance detected for the 7th time after 900 days, each is organized semen armeniacae amarae medicine materical crude slice and surveys amarogentin content and put front 2.69% in storage and compare, and all has reduction, and showing to preserve semen armeniacae amarae medicine materical crude slice after 900 days has had denaturalization phenomenon.
The 9th group of (ox-hide haptogen paper bag wherein, sealing, refrigeration), the 15th group (aluminium foil/vinyon compound membrane bag, sealing, refrigeration), the 12nd group (aluminium foil/vinyon compound membrane bag, vacuum, refrigeration), the 3rd group (polyethylene plastic bag, vacuum, refrigeration) changes minimum.Other each group all reduces more.
3.7.8 microorganism detection
According to 2010 editions Chinese pharmacopoeia appendix X III C limit test of microbe methods, check, result is as table 39.
The 7th maintenance of table 39 detects semen armeniacae amarae medicine materical crude slice microorganism detection result
Above result is known, preserves after 30 months, respectively to organize semen armeniacae amarae medicine materical crude slice microbial limit and all meet medicinal standard.
3.7.9 Analysis of test results
The storage of semen armeniacae amarae medicine materical crude slice warehouse-in, after 900 days, detects for the 7th time that carries out semen armeniacae amarae medicine materical crude slice maintenance test, passes through to detect semen armeniacae amarae medicine materical crude slice peroxide value, amarogentin content and appearance character comprehensive evaluation, substitution formula in test:
Comprehensive evaluation index=A i/ 2*0.1+0.005401/B i* 0.4+C i* 0.5
(A iocular estimate; B iperoxide value; C iamarogentin content)
Score value is higher shows that semen armeniacae amarae medicine materical crude slice storage effect is better, as shown in figure 19.
Test shows respectively to organize before semen armeniacae amarae prepared slice quality is put in storage all decline, wherein the 9th group (ox-hide haptogen paper bag, sealing, refrigeration), the 15th group (aluminium foil/vinyon compound membrane bag, sealing, refrigeration), the 3rd group of (polyethylene plastic bag, vacuum, refrigeration) variation minimum.Mass change is minimum, and storage effect is best; The 1st group of (polyethylene plastic bag packing, sealing, cool place) storage effect is the poorest.
Maintenance effect is followed successively by the 1st group of the 4th group of > blank group > of the 7th group of > of the 13rd group of > of the 8th group of > of the 5th group of > of the 11st group of > of the 14th group of > of the 10th group of > of the 2nd group of > of the 6th group of > of the 12nd group of > of the 3rd group of > of the 15th group of > of the 9th group of > of maintenance.
3.8 semen armeniacae amarae medicine materical crude slice packing storage experiment interpretations of result
3.8.1 putting 30 months semen armeniacae amarae medicine materical crude slice storage experiment results in storage comprehensively analyzes
To in early October, 2013, semen armeniacae amarae medicine materical crude slice storage maintenance 30 totally months, detects 7 times, and wherein top-quality group respectively: detection for the second time, the 7th, six, ten and five groups; Detect for the third time the tenth, two, five and 11 groups; Detect the 3rd, two, six and seven groups for the 4th time; Detect the tenth, 15, nine and six group for the 5th time; Detect the 3rd, nine, 15 and two groups for the 6th time; Detect the 3rd, nine, 15,12 and six groups for the 7th time.Each testing result is arranged and is all changed.Every group of semen armeniacae amarae medicine materical crude slice detected to gained comprehensive evaluation substitution formula for six times:
Maintenance effect=∑ E i(E comprehensive evaluation; I=2,3,4,5,6)
As shown in figure 20, the good and bad degree of semen armeniacae amarae medicine materical crude slice storage maintenance effect is followed successively by: the 4th group of the 14th group of > of the 13rd group of > of the 5th group of > of the 7th group of > of the 16th group of > of the 8th group of > > of the 1st group of > of the 11st group of > of the 12nd group of > of the 6th group of > of the 10th group of > of the 2nd group of > of the 15th group of > of the 9th group of > of the 3rd group of >.
3.8.2 semen armeniacae amarae medicine materical crude slice is packed storage experiment result quadrature analysis
The 7th semen armeniacae amarae medicine materical crude slice storage detected to experimental results list, use SPSS19.0 to carry out quadrature analysis, shown in table 40.
Form 40 semen armeniacae amarae medicine materical crude slice maintenance quadrature analysis
By table 40, can be obtained:
(1) each factor affects size and is followed successively by: B > C > A, be temperature > oxygen > packing, temperature is for affecting the greatest factor of the storage maintenance of semen armeniacae amarae medicine materical crude slice, secondly be the impact of oxygen, the impact of packing is minimum.
(2) III > II > I in three levels of temperature factor, low temperature is the best reserve temperature of semen armeniacae amarae medicine materical crude slice, is secondly that shady and cool environment, room temperature storage are the poorest.
(3) impact of oxygen is II > I, and under oxygen free condition, storage is better than preserving under aerobic conditions.
The impact of (4) three kinds of packings is III > II > I, and storage effect ox-hide haptogen paper bag is best, and secondly, polyethylene plastic bag is the poorest for aluminium foil/vinyon compound membrane bag.
(5) wherein best storage maintenance scheme is: because ox-hide haptogen paper bag cannot vacuum packaging, so best storage maintenance scheme is the vacuum packaging of foil laminated film bag packing, low temperature is preserved.
The Primary Study of 3.9 packing and the experiment of semen armeniacae amarae medicine materical crude slice compatibility
According to the report pharmaceutical packing material of Wang Xiaoyu [110] etc., to guaranteeing stability of drug products, play an important role, its quality will directly affect safe and effective for medication.Drug packing material composition, formula, selected supplementary material and production technology are different, cause incorrect material to cause that chemical reaction even occurs for the migration of active component, absorption, make drug failure or produce serious side effects, therefore require medicine to select before packing container, must fully evaluate its impact on medicine stability, carry out compatibility test.This experimental selection polyethylene (PE, Polyethylene) plastic film, ox-hide haptogen paper, 3 kinds of packing of aluminium foil/vinyon compound membrane bag carry out sealed package to semen armeniacae amarae medicine materical crude slice, vinyon monofilm is packaged in normal temperature, shady and cool, refrigerate under three kinds of conditions, other two kinds are packaged under shady and cool constant temperature, to preserve after 18 months and take out, take packing and drug compatibility as point of penetration, use GC-MS method to measure 3 kinds of blank packing, 3 kinds of organic residues in packing and 6 kinds of packaged semen armeniacae amarae medicine materical crude slice, and with reference to YBB00132002 composite membrane for packaging medicine, bag general rule and GB9685-94 food containers, packing are used in hygienic standard the regulation of the maximum use amount of additive are compared to research with additive, explore Different Package material and the difference of medicinal material on organic residue.
3.9.1 packing and the constituent analysis of semen armeniacae amarae medicine materical crude slice
3.9.1.1 instrument and test condition
HP6890/5973GC-MSD gas chromatograph-mass spectrometer; Chromatographic column HP-5MS, 30m*0.25mm*0.25um quartz capillary column; Carrier gas is helium, flow velocity 1.0ml/min.Sample size is 1 μ L, and split ratio is 10:1.260 ℃ of vaporizing chamber temperature, interface temperature is 260 ℃; Temperature programme: 60 ℃ of initial temperatures, 10 ℃ of per minutes rise to 290 ℃.Mass spectrum condition: 230 ℃ of ion source temperatures, quadrupole rod: 150 ℃, ionization mode: electron ionization (EI) mode, electron energy 70eV, scanning range 20-450M/Z.
3.9.1.2 sample and measuring method
Get the about 2.0g of semen armeniacae amarae sample (30 order) of each chopping, accurately weighed, adopt headspace solid-phase microextraction, 80 ℃ of head space temperature, head space time 40min; Draw 1 μ L sample introduction, record chromatlog.6 kinds of packing are shredded into the fragment that is less than 1mm, be placed in 20ml headspace sampling bottle; Guarantee that packing and semen armeniacae amarae medicinal material, at headspace sampling bottle same volume place, seal head space sample injection bottle immediately, carry out chromatographic analysis, sample grouping situation is in Table 41.
Table 41 sample grouping situation
3.9.1.3 results and analysis
Adopt headspace sampling-gas chromatography-mass spectrography to measure volatile organic matter in packing and semen armeniacae amarae, obtain gas chromatogram, identify the possible structure of each volatile ingredient, with peak area normalization method, calculate the relative content of each composition, corresponding mass spectrogram is retrieved and as calculated in conjunction with literature survey.
3.9.1.3.1 the composition of volatile organic matter in Different Package material and semen armeniacae amarae
Each sample organic residue Components identification result and relatively percentage composition are in Table 42.
The composition of volatile organic matter in table 42 packing and semen armeniacae amarae medicine materical crude slice
Note: "-" represents trace or do not contain this thing; BHT (antioxidant): dibutyl hydroxy toluene; BHA (antioxidant): butylated hydroxy anisole
3.9.1.3.2 result
From GC-MS qualification result, can find out, in each sample, organic residue is mainly fatty acid, aldoketones and oxidation terpenoid, is secondly benzene class material, alkanes and other aromatics.
Blank ox-hide haptogen paper bag detects and identifies 51 compositions altogether, wherein aldehyde C-9, hexanal, enanthaldehyde, capraldehyde, (±)-citrene, octanone, (±)-longicyclene, longifolene, tetradecane, 12 carbon alkane, syringyl alcohol, 2,5-bis-bromo-1,4-benzoquinones (2,5-cyclohexadiene-1,4-dione), antioxidant BHA (butylated hydroxy anisole, Butyl hydroxyanisd), antioxidant BHT (dibutyl hydroxy toluene, Butylated hydroxytoluene) is main component; The semen armeniacae amarae medicine materical crude slice ox-hide haptogen paper bag of 18 months is housed and detects altogether and identify 9 compositions, wherein hydrocyanic acid, benzaldehyde, pentadecane, acetic acid, phenmethylol are main component.
Blank polyethylene plastic bag detects and identifies 26 compositions altogether, and wherein ethanol, acetone, acetic acid, 2-furancarboxylic acid, (±) citrene, benzaldehyde, phenmethylol, hexane, aldehyde C-9, capraldehyde, borneol, (+)-longicyclene, longifolene, 12 carbon alkane, 2-methoxy-4-vinylphenol, naphthalene, antioxidant BHT are main component; Under shady and cool environment and under normal temperature environment, the semen armeniacae amarae medicine materical crude slice polyethylene plastic bag of 18 months is housed and all detects and identify 5 compositions, wherein hydrocyanic acid, ethanol, benzaldehyde, phenmethylol are main component.The semen armeniacae amarae medicine materical crude slice polyethylene plastic bag of 18 months is housed under cold storage environment and detects altogether and identify 8 compositions, wherein hydrocyanic acid, ethanol, benzaldehyde, phenmethylol, tetradecane, pentadecane are main component.
Blank aluminium foil/vinyon compound membrane bag detects and identifies 41 compositions altogether, wherein 2,2,3-trimethyl decane, furfural, 2,5-dimethyl 12 carbon alkane, 3-methylene-heptane, aldehyde C-9,2-furancarboxylic acid, (±)-citrene, 12 carbon alkane, tetradecane, 2,2,5,5-tetramethyl hexane, 4-ethyl-2,2,6,6-tetramethyl heptane, (E)-4-octenal, octanal, phenylacetaldehyde, capraldehyde, caprolactam, antioxidant BHT are main component; Semen armeniacae amarae medicine materical crude slice aluminium foil/vinyon compound membrane bag of 18 months is housed and detects altogether and identify 7 compositions, wherein hydrocyanic acid, ethanol, benzaldehyde, phenmethylol, caprolactam are main component.
The Different Package material packing semen armeniacae amarae medicine materical crude slice of 18 months, adopts the semen armeniacae amarae medicine materical crude slice of ox-hide haptogen paper bag packing to detect altogether and identify 7 compositions, and wherein hydrocyanic acid, acetic acid, benzaldehyde, phenmethylol, 4-isopropyl toluene are main component; Under shady and cool environment with under normal temperature environment, adopt the semen armeniacae amarae medicine materical crude slice of polyethylene plastic bag packing to detect altogether and identify 7 compositions, wherein hydrocyanic acid, ethanol, benzaldehyde, phenmethylol, 3-phenyl-2-acrolein are main component; The semen armeniacae amarae medicine materical crude slice polyethylene plastic bag of 18 months is housed under cold storage environment and detects altogether and identify 6 compositions, wherein hydrocyanic acid, ethanol, benzaldehyde, phenmethylol, 1-hydroxyl-1-phenyl-2-acetone are main component.Adopt the semen armeniacae amarae medicine materical crude slice of aluminium foil/vinyon compound membrane bag packing to detect altogether and identify 6 compositions, wherein hydrocyanic acid, ethanol, benzaldehyde, phenmethylol, 1-phenyl-1,2-propanedione is main component.
3.9.1.3.3 brief summary and discussion
3.9.1.3.3.1 the comparison of organic residue before and after Different Package material packing
Different Package material is carried out to GC-MS comparative analysis, volatile solvent acetone, 1, 6, 6-trimethyl-cyclohexene is peculiar by blank polyethylene plastic bag, isopropyl alcohol, n-amyl alcohol, enanthaldehyde, 3-octanone, nonyl alcohol, 3, 5-orcin, linalool, hendecene, sad, 2, 3-dihydro-benzofuran, cyclotetradecane, geranyl acetone, butylated hydroxy anisole (antioxidant BHA), heptadecane, syringyl alcohol, dihydroactinidiolide, 3-methyl-3-cyclohexen-1-ol, by blank ox-hide haptogen paper bag peculiar, be equipped with in the semen armeniacae amarae medicine materical crude slice ox-hide haptogen paper bag of 18 months and polyethylene plastic bag and all contain hydrocyanic acid, acetic acid, benzaldehyde, phenmethylol, longifolene, 1-phenyl-1, 2-propanedione, 1-hydroxyl-1-phenyl-2-acetone.
Conventional additive antioxidants BHT and BHA Chang Bingyong in plastic package material, and all have certain toxicity.BHT all contains in three kinds of blank packing, and BHA only contains in blank ox-hide haptogen paper bag, but does not detect in medicinal material [110].
By noxious residual chemicals in three kinds of packing is compared, show that polyethylene plastic bag is more suitable for the packing of semen armeniacae amarae medicine materical crude slice.
3.9.1.3.3.2 the impact of Different Package material on semen armeniacae amarae medicine materical crude slice
Semen armeniacae amarae medicine materical crude slice to different packaging material packings carries out GC-MS analysis, and wherein hydrocyanic acid, benzaldehyde, phenmethylol, 1-hydroxyl-1-phenyl-2-acetone are the main component of 18 months semen armeniacae amarae medicine materical crude slice of packing storage; Infer that hydrocyanic acid is because the amarogentin hydrolysis in semen armeniacae amarae is relevant with benzaldehyde.The semen armeniacae amarae of employing Different Package material storage becomes to be grouped into also difference, visible, Different Package material is larger on the impact of organic substance residues in medicine materical crude slice composition, and in Different Package material and semen armeniacae amarae medicine materical crude slice, the quantitative relationship of noxious residual chemicals is worth further research.
4. conclusion and discussion
4.1 conclusion
4.1.1 semen armeniacae amarae medicine materical crude slice storage maintenance is 30 months, detect seven times, pass through comprehensive grading, the good and bad degree of semen armeniacae amarae medicine materical crude slice storage maintenance effect is followed successively by: the 4th group of the 14th group of > of the 13rd group of > of the 5th group of > of the 7th group of > of the 16th group of > of the 8th group of > > of the 1st group of > of the 11st group of > of the 12nd group of > of the 6th group of > of the 10th group of > of the 2nd group of > of the 15th group of > of the 9th group of > of the 3rd group of >.
4.1.2 according to the results of analysis of variance, the greatest factor of semen armeniacae amarae medicine materical crude slice storage maintenance is temperature, and wherein low temperature is best, and secondly shady and cool, normal temperature is the poorest; Next is having or not of oxygen, and anaerobic is better than aerobic; Then be packing, its heifer haptogen paper bag best (but can not vacuumize), is secondly aluminium foil/vinyon compound membrane bag, is finally polyethylene plastic bag.
4.1.3 moisture is always all at the safe aqueous ingredients of medicine materical crude slice below 13.0%.In illustrative experiment, various packing storage practices all can play moistureproof effect.
Low variation when 4.1.4 although peroxide value is high while presenting in experiment, to be that the peroxide that produces in Oxidation of Fat and Oils process is unstable very easily decompose and cause in supposition, measures all in the specialized range of pharmacopeia at every turn.
4.1.5 because semen armeniacae amarae may occur mouldy denaturalization phenomenon in storage, the safety of medication and validity generation are had a strong impact on, therefore carried out the detection of germ, detect with reference to containing the standard of medicinal powder, all composite demand in the oral formulations of similar instructions of taking in 2010 editions Chinese pharmacopoeia.
4.1.6 the inner wrapping prepared slices of Chinese crude drugs move towards modern significant to Chinese medicine, have overcome the problems such as pollution, efficiency in " hand is grabbed and weighed with a small steelyard title " is low.But it is uncertain whether packing have impact and affect size medicinal material, we carry out the research of the compatibility of packing and semen armeniacae amarae medicine materical crude slice for this reason, show that in packing, polyethylene plastic bag is better than aluminium foil/vinyon compound membrane bag, aluminium foil/vinyon compound membrane bag is better than ox-hide haptogen paper bag.
Although 4.1.7 ox-hide haptogen paper bag is optimum in the statistics of influence factor, in conjunction with compatibility experimental result, its volatility composition is maximum, and comprehensive front and back factor, show that best packing are aluminium foil/vinyon compound membrane bag.Best storage protocol is: the vacuum packaging of aluminium foil/vinyon compound membrane bag, the storage of cold place.
4.2 discuss
Peroxide value means peroxide and potassium iodide effect in grease, generates the percentum of free-iodine.Peroxide is the intermediate product in Oxidation of Fat and Oils process, it is one of toxic substance of grease generation, it is one of important sensitive indicator of judgement Oxidation of Fat and Oils, bad change, not only several kinds of Chinese medicinal materials be take it as index of quality, also often application in actual production, as the quality testing of rapeseed oil, lard, peanut wet goods.
The principle of determination of POV is that peroxide reflection contained in hydroiodic acid and grease can be separated out iodine, within containing the reagent of glacial acetic acid, add potassium iodide can obtain hydroiodic acid, with sodium thiosulfate standard solution titration iodine, according to its consumption, can obtain peroxide value.But in peroxide value testing process, be subject to various factors, cause test error bigger than normal, so will be in strict accordance with requiring operation in experimentation, must be now with the current as saturated solution of potassium iodide, starch indicator, other reagent methenyl choloride, glacial acetic acid, detection water all will detect before experiment.
In this experiment, peroxide value is always all in the specialized range of pharmacopeia, but time low when high, the temperature while inferring with storage changes relevant with inherent substance reaction.

Claims (1)

1. a packing storage practice for semen armeniacae amarae medicine materical crude slice, it comprises the steps:
A, semen armeniacae amarae medicinal material is gathered after, qualified semen armeniacae amarae medicine materical crude slice is concocted in processing;
B, the vacuum packaging of employing aluminium foil/vinyon compound membrane bag, the storage of cold place.
CN201410213198.1A 2014-05-20 2014-05-20 Package and storage method of bitter almond kernel decoction piece Pending CN103950640A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410213198.1A CN103950640A (en) 2014-05-20 2014-05-20 Package and storage method of bitter almond kernel decoction piece

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410213198.1A CN103950640A (en) 2014-05-20 2014-05-20 Package and storage method of bitter almond kernel decoction piece

Publications (1)

Publication Number Publication Date
CN103950640A true CN103950640A (en) 2014-07-30

Family

ID=51328036

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410213198.1A Pending CN103950640A (en) 2014-05-20 2014-05-20 Package and storage method of bitter almond kernel decoction piece

Country Status (1)

Country Link
CN (1) CN103950640A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115169751A (en) * 2022-09-02 2022-10-11 张家港市绿色中药饮片有限公司 Method and system for improving maintenance quality of traditional Chinese medicine decoction pieces

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3958391A (en) * 1974-11-21 1976-05-25 Kabushiki Kaisha Furukawa Seisakusho Vacuum packaging method and apparatus
CN101084931A (en) * 2007-06-28 2007-12-12 临沂泰豪国际贸易有限公司 System and method for compounding boiled-free traditional Chinese medicine decoction pieces
CN201612831U (en) * 2009-12-04 2010-10-27 何沣原 Vacuum Chinese medicine herbal tablet packaging bag
CN102085152A (en) * 2009-12-04 2011-06-08 何沣原 Packaging bag for sealing Chinese medicinal decoction pieces
CN202236280U (en) * 2011-07-28 2012-05-30 丁永峰 Traditional Chinese medicinal slice package
CN203282772U (en) * 2013-05-14 2013-11-13 常州市华健药用包装材料有限公司 Composite film for drug packing bag

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3958391A (en) * 1974-11-21 1976-05-25 Kabushiki Kaisha Furukawa Seisakusho Vacuum packaging method and apparatus
CN101084931A (en) * 2007-06-28 2007-12-12 临沂泰豪国际贸易有限公司 System and method for compounding boiled-free traditional Chinese medicine decoction pieces
CN201612831U (en) * 2009-12-04 2010-10-27 何沣原 Vacuum Chinese medicine herbal tablet packaging bag
CN102085152A (en) * 2009-12-04 2011-06-08 何沣原 Packaging bag for sealing Chinese medicinal decoction pieces
CN202236280U (en) * 2011-07-28 2012-05-30 丁永峰 Traditional Chinese medicinal slice package
CN203282772U (en) * 2013-05-14 2013-11-13 常州市华健药用包装材料有限公司 Composite film for drug packing bag

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张丽娟: "苦杏仁小包装饮片贮藏养护研究", 《中国硕士学位论文全文数据库医药卫生科技》, 30 April 2013 (2013-04-30) *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115169751A (en) * 2022-09-02 2022-10-11 张家港市绿色中药饮片有限公司 Method and system for improving maintenance quality of traditional Chinese medicine decoction pieces

Similar Documents

Publication Publication Date Title
CN102150704B (en) Fruit and vegetable fresh-keeping agent and preparation method thereof
Huang et al. Comparison of HS-SPME with hydrodistillation and SFE for the analysis of the volatile compounds of Zisu and Baisu, two varietal species of Perilla frutescens of Chinese origin
Oyourou et al. Purification, stability and antifungal activity of verbascoside from Lippia javanica and Lantana camara leaf extracts
Xiao et al. Improved method to obtain essential oil, asarinin and sesamin from Asarum heterotropoides var. mandshuricum using microwave-assisted steam distillation followed by solvent extraction and antifungal activity of essential oil against Fusarium spp
Mpho et al. Use of lemongrass oil and modified atmosphere packaging on control of anthracnose and quality maintenance in avocado cultivars
Aghassi et al. Chemical composition of the essential oil of Cyperus rotundus L. from Iran
CN103083366A (en) Glossy ganoderma-lentinus edodes stem solid state fermentation compound as well as preparation method and application thereof
Wu et al. A novel application of the vacuum distillation technology in extracting Origanum vulgare L. essential oils
CN103266015A (en) Natural aromatic essential oil acquisition apparatus and application method
Kamatou et al. Headspace analysis and characterisation of South African propolis volatile compounds using GCxGC-ToF-MS
Marandi et al. Improving postharvest quality of table grape cv.“rish baba” using Thymus kotschyanus and Carum copticum essential oils
Bhandari et al. 1, 8-Cineole: A predominant component in the essential oil of large cardamom (Amomum subulatum Roxb.)
Liu et al. Characterization of ganoderma spore lipid by stable carbon isotope analysis: implications for authentication
Price et al. Stress metabolite production in potato tubers infected by Phytophthora infestans, Fusarium avenaceum and Phoma exigua
CN102764299B (en) Extraction method of traditional Chinese medicinal materials
CN103950640A (en) Package and storage method of bitter almond kernel decoction piece
CN103235058A (en) Method for measuring combined-state aroma substances in cereal raw materials for food brewage
CN105548391A (en) Method for detecting residues of organochlorine and pyrethrin at different positions in vegetables
CN103950638A (en) Sealwort decoction piece packaging and storing method
CN105596397B (en) A kind of fermentation Rhizoma Atractylodis Macrocephalae and its preparation method and application
CN107271582A (en) The detection method of citrinin toxin in a kind of red yeast rice
CN104042635B (en) A kind of cockroach medicinal tablets and preparation method thereof
CN104207975B (en) A kind of perfume with anophelifuge bacteriostasis efficacy and preparation method thereof
CN105920365A (en) Manufacturing method of Dendrobium nobile wall-broken powder
CN108828107A (en) A kind of gas chromatography combined with mass spectrometry method detecting the scented rice true and false

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20140730