CN106706634A - Quality standard and preparation process of qualitative and quantitative Chinese herbal astragali radix decoction slice - Google Patents
Quality standard and preparation process of qualitative and quantitative Chinese herbal astragali radix decoction slice Download PDFInfo
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Abstract
The invention provides a safe, efficient and convenient Chinese herbal astragali radix decoction slice. The invention provides a preparation process of a qualitative and quantitative Chinese herbal astragali radix decoction slice. By a processing technology, the astragali radix meeting a quality standard is prepared into the Chinese herbal decoction slice with the thickness of 0.3-1 mm, and the Chinese herbal decoction slice can be taken after being brewed, so that the conventional decocting and taking method is changed. The invention also provides the quality standard of the astragali radix decoction slice. On the basis of the existing quality standard, relevant test items are added and standard limits of astragaloside A and calycosin-7-glucoside during content determination are increased, so that the quality of the astragali radix decoction slice can be effectively controlled, the quality standard of a drug is enhanced, and the safety of drug application is improved.
Description
Technical field
The present invention relates to the field of Chinese medicines, the specially quality standard of the Radix Astragali qualitative, quantitative prepared slices of Chinese crude drugs, operational procedure and system
Make technique.
Background technology
The Radix Astragali (scientific name：Astragali radix), also known as continuous stilbene, astragalus, only mulberry, another name for Sichuan Province fat, hundred, hundred absorbent cotton, Huang Can,
Blood ginseng, people's rank, are the dry root of legume astragalus mongholicus Bge or Astragalus membranacus.Radix Astragali original name astragalus, history is loaded in《Legendary god of farming's book on Chinese herbal medicine
Through》, it is classified as top grade.Li Shizhen (1518-1593 A.D.) is released its name and is said：" over sixty years of age, long, astragalus color is yellow, is the length of tonic, therefore named.", show the Radix Astragali for me
One of Qi-tonifying drug that state is always most praised highly, taking this medicine can make one good health and a long life.Lu Yanqi, He Xueli's《Radix Astragali research is existing
Shape》It is comprehensive in terms of Radix Astragali biological characteristics, plant resources, karyotype, active chemical, pharmacological action etc. to discuss yellow
Stilbene research and development and is described in detail containing Multiple components such as polysaccharide, saponin(e, flavones in the Radix Astragali using the progress of aspect, and is mentioned
The Radix Astragali contains other compositions：Amino acids, trace element, sterols, folic acid, leukotrienes, linoleic acid etc..The Radix Astragali is used as conventional
Chinese medicine, with powerful potentiality to be exploited.
Current edition《Chinese Pharmacopoeia》Record, the function of the Radix Astragali with cure mainly for：Tonifying Qi and lifting yang, strengthening exterior and reducing sweat, inducing diuresis for removing edema is raw
Tianjin blood-nourishing, the stagnant logical numbness of row, pus draining and toxin expelling, expelling pus and promoting granulation.For treatment deficiency of vital energy weak, anorexia and loose stool, the sinking of qi of middle-jiao, rush down prolapse of the anus for a long time, just
Metrorrhagia is leaked, exterior deficiency spontaneous perspiration, deficiency of vital energy oedema, Heat Diabetes, blood deficiency chlorosis, hemiplegia, and numbness pain is numb, ulcer is difficult to burst, is burst long not
Hold back.Cai Li, Zhu Jiang's etc.《Astragalus polyose present Research and progress》In show that substantial amounts of clinical trial shows that astragalus polyose has
Regulation immunity of organisms reaches antineoplastic action.The prepared slices of Chinese crude drugs are the parts that Chinese medicine industry can not be lacked, and are TCMs
Bed is dialectical to treat required traditional weapon, the curative effect that its quality directly affects tcm clinical practice diseases prevention, cures the disease, otherwise for modern
Quick rhythm of life, high-quality that the present invention is provided, can brew and take the prepared slices of Chinese crude drugs for changing traditional decoction instructions of taking and have
The larger market demand.
Combination of Chinese tradiational and Western medicine magazine was once carried out in the 6th phase of volume 9 in 1989《The clinical practice of the Radix Astragali and research》Seminar,
Think that the Radix Astragali, as traditional traditional tonic medicine simply, with the effect such as QI invigorating, qi-restoratives, rising Yang, solid table, pus draining and toxin expelling, is such as carried in text
And " ginseng stilbene is of the same name, but common people's ' recognize ginseng and do not recognize stilbene ', someone says that real expert seemingly ' recognizes stilbene and do not recognize ginseng ', because the Radix Astragali is used
Way is wider." Radix Astragali purposes is extensive certainly, clinical practice is in antitumor, antiviral, promoting immunity, the anti-ageing, diuretic antihypertensive of health care etc.
Aspect, it is effective in cure to treatment hyperthyroidism, tuberculosis, climacteric night sweat, diabetes, chronic inflammation etc..It is worth noting that, in text
The money of BJ Union Hospital from put forth energy chief physician mention " in clinical practice, Radix Astragali consumption is critically important, I typically commonly use 30~
60g.Current problem be the quality and concocting method of the Radix Astragali it cannot be guaranteed that, usually affect the treatment." to be solved by this invention ask
Topic is to solve the problems such as generally existing The Quality of Sliced Herbal Medicine in the market is not up to standard, curative effect is not obvious.
Brief description of the drawings
Accompanying drawing 1 is Radix Astragali qualitative, quantitative Manufacture of medicinal slices of TCM process chart.
The content of the invention
In order to solve the above problems, quality standard and the manufacture work of the Radix Astragali qualitative, quantitative prepared slices of Chinese crude drugs that the present invention is provided
Skill, increases medicine bits impurity, AFB1, sulfur dioxide residual quantity, and improve the standard of Astragaloside IV in assay
Limit is improved to 0.044% from 0.040%, the standard limits of calycosin glucoside from 0.020% improve to
0.022%.And the Radix Astragali prepared slices of Chinese crude drugs of 0.3~1mm of slice thickness are produced by specific operation, it is ensured that the prepared slices of Chinese crude drugs meet height
The requirement of standard high-quality.
The manufacturing process of the Radix Astragali qualitative, quantitative prepared slices of Chinese crude drugs that the present invention is provided, comprises the following steps：
A10 net systems：The impurity that is mixed in the Radix Astragali of removing and the product that go mouldy etc., or the Radix Astragali is carried out into stepping by size, to reach
To clean or be processed further treatment.Note：The Radix Astragali must not directly contact ground after cleaning.
A20 demulcens：The Radix Astragali after net system is put into medicine processing device, demulcen 20min-1h under vacuum negative pressure condition, thorough to the Radix Astragali
Bottom runs through, and plane of rupture is without the dry heart.Demulcen parameter：55-60 DEG C of temperature, pressure -0.05MPa, spray time 1s spray time delay
100s.Note：The Radix Astragali need to run through, and plane of rupture is soft or hard suitable inside and outside the Radix Astragali without the dry heart.
A30 cuttings：Piece 0.3~1mm of thickness, is operated by fully automatic high-speed slicer operational procedure, mixes up knife away from the Radix Astragali is entered
Row trial cut, is detected with slide measure, adjusts cutting thickness, formally cuts medicine after meeting the requirements again.
A40 is dried：It is dried using heated-air circulation oven, Radix Astragali material is laid on baking oven shelf, paving thickness is uniform,
Thickness is in below 3cm.Switch is opened, heater switch, blower fan is opened, 50 ± 2 DEG C are dried in temperature, and setting is reached in temperature
3-4h is dried after temperature, drying is finished, and closes heater switch, continue to dry, treat that the temperature inside the box is fallen to 35~40 DEG C, close wind
Machine.Post personnel need to fill in intermediate products and please examine list after drying, hand over Quality Mgmt Dept to carry out moisture inspection by QA samplings.
A50 is packed：Packed according to the requirement of this product packing specification.Need to check make-up room before packaging, confirm bag
Clearing out a gathering place for assembling production lines has been completed, and checks whether packaging material meet the requirements.Inner packing：Being adjusted in equipment needs print
The date of manufacture of system, lot number, QA monitoring, the Radix Astragali for weighing predetermined weight are put into hopper, are sealed with sealing machine, it is desirable to accomplish envelope
Mouth is tight, smooth, attractive in appearance.External packing：Adjusted in equipment the date of manufacture and lot number that need to be printed, QA monitoring, in external packing
Lot number, date of manufacture are printed on box, should be noted whether lot number and date of manufacture are clear in print procedure.After the completion of inner packing
Medicine materical crude slice and survey report be put into outsourcing box, 4 bags/box.Every 10 box medicine materical crude slice is inserted in 1 heat shrinkage film, carries out hot receipts
Contracting；It is fitted into after thermal contraction in big carton, 240 boxes/case.In operating process, QA is inspected by random samples at any time.Post personnel need to fill in into after packaging
Product please examine list, hand over Quality Mgmt Dept to carry out product examination by QA samplings.
A60, finished product：Post personnel need to fill in finished product and please examine list after packaging, hand over Quality Mgmt Dept to carry out product examination by QA samplings.
Increase medicine bits impurity, AFB1, sulfur dioxide residual quantity, and improve Astragaloside IV in assay
Standard limits are improved to 0.044% from 0.040%, the standard limits of calycosin glucoside from 0.020% improve to
0.022%.The quality standard of the revised Radix Astragali qualitative, quantitative prepared slices of Chinese crude drugs is as follows：
Radix Astragali medicine materical crude slice
Phonetic title：Huangqi Yinpian
Packaging：Fine aluminium composite film packaging.
【Proterties】Take this product appropriate, observe in the sunlight, in similar round or the piece of ellipse, exocuticle yellow-white is extremely for this product
Light brown brown, tangent plane skin zone yellow-white, woody part is faint yellow, there is radial texture and crack.It is smelt, fragrance is little, taste it, it is micro-
It is sweet, have beany flavor.
Differentiate
Microscopical characters
Instrument and apparatus：Medicinal herb grinder, pharmacopeia sieve, microscope, alcolhol burner
Reagent and test solution：(reagent is used and divided for chloraldurate test solution, glycerine acetic acid test solution, glycerol-alcohol test solution, dilute glycerine
Analysis is pure, and experimental water is purified water)
Determine and result judgement：In right amount, picking is put on slide a little, and glycerine vinegar is added dropwise to take this product powder (crossing No. four sieves)
Sour test solution, chloraldurate test solution or other test solutions 1~2 drop, covered.After chloraldurate test solution is added dropwise if necessary, in wine
Saturatingization is heated on smart lamp, and glycerol-alcohol test solution or dilute glycerine, covered, in basis of microscopic observation is added dropwise：Powder is yellowish-white
Color.Fiber bunchy is dissipated from there is longitudinal crack on 8~30 μm of diameter, wall thickness, surface, and primary wall is often separated with secondary wall, two ends normal off
Palpus shape is cleaved into, or it is more truncate.Bordered pit vessel is colourless or orange-yellow, and bordered pit arrangement is tight.Lithocyte is rare, circular,
Long Circle is in irregular shape, and wall is thicker.
Thin layer differentiates
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, supersonic wave cleaning machine, thermostat water bath, sample applicator,
Expansion cylinder, lamellae, three use ultraviolet device
Reagent and test solution：Methyl alcohol, neutral alumina, water-saturated n-butanol, chloroform, sulfuric acid, ethanol, NaOH,
Watery hydrochloric acid, ethyl acetate, anhydrous sodium sulfate, ammonia (reagent is pure using analysis, and experimental water is purified water)
Control medicinal material and reference substance：Radix Astragali control medicinal material, Astragaloside IV reference substance
Take this product powder 3g, plus methyl alcohol 20ml, be heated to reflux 1 hour, filter, filtrate be added on neutral alumina column (100~
120 mesh, 5g, internal diameter is 10~15mm) on, eluted with 40% methyl alcohol 100ml, eluent is collected, it is evaporated, the residue 30ml that adds water makes
Dissolving, is shaken with water saturated n-butanol and extracted 2 times, and each 20ml merges n-butanol liquid, washes with water 2 times, each 20ml,
Aqueous are discarded, n-butanol liquid is evaporated, residue adds the methyl alcohol 0.5ml to make dissolving, used as need testing solution.It is another to take Astragaloside IV control
Product, plus methyl alcohol is made solution of every 1ml containing 1mg, used as reference substance solution.According to thin-layered chromatography (general rule 0502) experiment, draw
Each 2 μ l of above two solution, put on same silica gel g thin-layer plate, with the lower floor of chloroform-methanol-water (13: 7: 2) respectively
Solution is solvent, is launched, and is taken out, and is dried, and is sprayed with 10% ethanol solution of sulfuric acid, is heated to spot development at 105 DEG C clear.Knot
Fruit judges：In test sample chromatogram, on position corresponding with reference substance chromatogram, identical sepia spot is shown under daylight；It is ultraviolet
Show the orange-yellow fluorescence spot of identical under light lamp (365nm).
This product powder 2g, plus ethanol 30ml are taken, is heated to reflux 20 minutes, filtered, filtrate is evaporated, and residue adds 0.3% hydrogen-oxygen
Changing sodium solution 15ml makes dissolving, filters, and filtrate adjusts pH value to 5~6 with watery hydrochloric acid, is shaken with ethyl acetate 15ml and extracted, point
Acetic acid ethyl fluid is taken, is filtered with the filter paper for being covered with appropriate anhydrous sodium sulfate, filtrate is evaporated.Residue adds the ethyl acetate 1ml to make dissolving,
As need testing solution.Radix Astragali control medicinal material 2g separately is taken, control medicinal material solution is made in the same way of.According to thin-layered chromatography (general rule 0502)
Experiment, draws each 10 μ l of above two solution, puts respectively on same silica gel g thin-layer plate, is with chloroform-methyl alcohol (10: 1)
Solvent, launches, and takes out, and dries, and puts after smoking in ammonia steam, puts and inspect under ultraviolet lamp (365nm).Result judgement：Test sample
In chromatogram, on position corresponding with control medicinal material chromatogram, show the fluorescence principal spot of same color.
Check
Medicine bits, impurity
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve
Determine and result judgement：Determined according to determination of foreign matter method (general rule 2301).
Test sample about 100g (being accurate to 0.1g) is taken, is spread out, sort out impurity, sifted out medicine with No. 6 and consider to be worth doing, merged, weighed, counted
Calculate its amount (%) in test sample.
Result judgement：This product medicine bits, impurity must not cross 3%.
Moisture
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, electric heating constant-temperature blowing drying box, measuring cup
Determine and result judgement：Determined according to aquametry (method of general rule 0,832 second).
2~5g of test sample is taken, is laid in and is dried into the flat measuring cup of constant weight, thickness is no more than 5mm, loose test sample
Accurately weighed no more than 10mm, open bottle cover covers bottle cap in 100~105 DEG C of dryings 5 hours, in dislocation drier, puts
It is cold 30 minutes, accurately weighed, then dried 1 hour in said temperature, let cool, weigh, it is no more than to the double difference weighed
Untill 5mg.According to the weight of less loss, water content (%) in test sample is calculated.
Result judgement：This product moisture must not cross 10.0%.
Total ash
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, Muffle furnace, electric furnace, crucible
Determined according to Ash determination method (general rule 2302).
2~3g of test sample (as acid-insoluble ash must be determined, can use 3~5g of test sample) is taken, the earthenware of ignition to constant weight is put
In crucible, weighed weight (accurately to 0.01g) is slowly red-hot, notes avoiding burning, when carbonizing completely, gradually rises temperature extremely
500~600 DEG C, make ashing completely and to constant weight.According to residue weight, the content (%) of total ash in test sample is calculated.
Result judgement：This product total ash must not cross 5.0%.
Heavy metal and harmful element
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, microwave dissolver, atomic absorption spectrophotometer
Reagent and test solution：Nitric acid, ammonium dihydrogen phosphate, magnesium nitrate, KI, ascorbic acid, hydrochloric acid, sodium borohydride, hydrogen-oxygen
(wherein nitric acid, ammonium dihydrogen phosphate, magnesium nitrate are top pure grade, and other reagents are used to change sodium, sulfuric acid, potassium permanganate, hydroxylamine hydrochloride
Analysis is pure, and experimental water is purified water)
Standard sample：Lead single element standard sample, cadmium single element standard sample, arsenic single element standard sample, mercury single element
Standard sample, copper single element standard sample
Method：Determined according to lead, cadmium, arsenic, mercury, copper determination method (general rule 2321)
The measure (graphite furnace method) of lead
Condition determination reference conditions：Wavelength 283.3nm, 100~120 DEG C of drying temperature continues 20 seconds；Ashing temperature 400
~750 DEG C, continue 20~25 seconds；Atomization temperature 1700~~2100 DEG C, continue 4~5 seconds.
The preparation precision of lead Standard Reserving Solution measures lead single element standard liquid in right amount, is diluted with 2% salpeter solution, is made
Per the solution of the μ g of 1ml leaded (Pb) 1, obtain final product (0~5 DEG C of storage).
Precision measures lead Standard Reserving Solution in right amount respectively for the preparation of standard curve, and every 1ml difference is made of 2% salpeter solution
The solution of leaded 0ng, 5ng, 20ng, 40ng, 60ng, 80ng.Precision measures 1ml respectively, precision plus containing 1% ammonium dihydrogen phosphate and
The solution 0.5ml of 0.2% magnesium nitrate, mixes, and precision draws 20 μ l injection graphite furnace atomizers, mensuration absorbance, with extinction
It is ordinate to spend, and concentration is abscissa, draws standard curve.
The preparation A methods of need testing solution take test sample meal 0.5g, accurately weighed, put in politef counteracting tank, plus
3~5ml of nitric acid, mixes, and soaked overnight covers inner cap, screws overcoat, put in suitable Hyperfrequency waves eliminating stove, cleared up (by instrument
What device specified clears up procedure operation).After clearing up completely, cancel solution inner canister and put and be slowly heated on electric hot plate rufous steam and wave
It is most, and continuation is slowly concentrated into 2~3ml, lets cool, and is transferred in 25ml measuring bottles with water, and scale is diluted to, shake up, obtain final product.Same method
While reagent preparation blank solution.
Determination method precision measures blank solution and each 1ml of need testing solution, and precision adds and contains 1% ammonium dihydrogen phosphate and 0.2%
The solution 0.5ml of magnesium nitrate, mixes, precision 10~20 μ l of absorption, method mensuration absorbance under the preparation of sighting target directrix curve, from
The content of lead (Pb) in need testing solution is read on standard curve, is calculated, obtained final product.
Cadmium detrmination (graphite furnace method)
Condition determination reference conditions：Wavelength 228.8nm, 100~120 DEG C of drying temperature continues 20 seconds；Ashing temperature 300
~500 DEG C, continue 20~25 seconds；1500~1900 DEG C of atomization temperature, continues 4~5 seconds.
The preparation precision of cadmium Standard Reserving Solution measures cadmium single element standard liquid in right amount, is diluted with 2% salpeter solution, is made
The solution containing the μ g of cadmium (Cd) 1 per 1ml, obtains final product (0~5 DEG C of storage).
Precision measures cadmium Standard Reserving Solution in right amount respectively for the preparation of standard curve, is diluted with 2% salpeter solution and is made every 1m1
The solution of 0ng containing cadmium, 0.8ng, 2.0ng, 4.0ng, 6.0ng, 8.0ng respectively.Accurate respectively to draw 10 μ l, injection graphite furnace is former
Sonization device, mensuration absorbance, with absorbance as ordinate, concentration is abscissa, draws standard curve.
The preparation of need testing solution determines the preparation of need testing solution under item with lead.
Determination method is accurate to draw blank solution and each 10~20 μ l of need testing solution, method under the preparation of sighting target directrix curve
Mensuration absorbance (if test sample has interference, precision can measure standard liquid, blank solution and each 1ml of need testing solution, essence respectively
Solution 0.5ml close plus containing 1% ammonium dihydrogen phosphate and 0.2% magnesium nitrate, mixes, and determines in accordance with the law), read from standard curve and supplied
The content of cadmium (Cd) in test sample solution, calculates, and obtains final product.
The measure (hydride method) of arsenic
Condition determination uses suitable hydride generation system, and (use is faced with containing sodium borohydride and 0.3% sodium hydroxide solution
Preceding preparation) used as reducing agent, hydrochloric acid solution (1 → 100) is carrier fluid, nitrogen is carrier gas, and Detection wavelength is 193.7nm.
The preparation precision of arsenic Standard Reserving Solution measures arsenic single element standard liquid in right amount, is diluted with 2% salpeter solution, is made
The solution containing the μ g of arsenic (As) 1 per 1ml, obtains final product (0~5 DEG C of storage).
Precision measures arsenic Standard Reserving Solution in right amount respectively for the preparation of standard curve, is diluted with 2% salpeter solution and is made every 1ml
The solution of 0ng containing arsenic, 5ng, 10ng, 20ng, 30ng, 40ng respectively.Precision measures 10ml respectively, in putting 25ml measuring bottles, plus
25% liquor kalii iodide (prepared before use) 1ml, shakes up, plus 10% ascorbic acid solution (prepared before use) 1ml, shakes up, and uses
Hydrochloric acid solution (20 → 100) is diluted to scale, shakes up, close plug, puts in 80 DEG C of water-baths and heats 3 minutes, takes out, and lets cool.Take in right amount,
Suction hydride generation system, determines absorption value, and with peak area (or absorbance) as ordinate, concentration is abscissa, draws mark
Directrix curve.
The preparation of need testing solution is prepared with the A methods in the preparation of need testing solution under lead measure item.
Determination method is accurate to draw blank solution and each 10ml of need testing solution, under the preparation of sighting target directrix curve, from " plus
25% liquor kalii iodide (prepared before use) 1ml " rises, and determines in accordance with the law.The arsenic (As) from need testing solution is read on standard curve
Content, calculate, obtain final product.
The measure (cold steam absorption process) of mercury
Condition determination uses suitable hydride generation system, with molten containing 0.5% sodium borohydride and 0.1% NaOH
Used as reducing agent, hydrochloric acid solution (1 → 100) is carrier fluid to liquid (prepared before use), and nitrogen is carrier gas, and Detection wavelength is 253.6nm.
The preparation precision of mercury Standard Reserving Solution measures mercury single element standard liquid in right amount, is diluted with 2% salpeter solution, is made
Per the solution of the μ g of 1ml mercurous (Hg) 1, obtain final product (0~5 DEG C of storage).
The preparation of standard curve respectively precision measure mercury Standard Reserving Solution 0ml, 0.1ml, 0.3ml, 0.5ml, 0.7ml,
0.9ml, in putting 50ml measuring bottles, plus 20% sulfuric acid solution 10ml, 5% liquor potassic permanganate 0.5ml, shake up, 5% hydrochloric acid hydroxyl is added dropwise
Amine aqueous solution to aubergine just disappears, and is diluted with water to scale, shakes up.Appropriate, suction hydride generation system is taken, is determined and is absorbed
Value, with peak area (or absorbance) as ordinate, concentration is abscissa, draws standard curve.
The preparation A methods of need testing solution take test sample meal 0.5g, accurately weighed, put in polytetrafluoroethylene (PTFE) counteracting tank, plus
3~5ml of nitric acid, mixes, and soaked overnight covers inner cap, screws overcoat, puts in suitable Hyperfrequency waves eliminating stove and cleared up (by instrument
What device specified clears up procedure operation).After clearing up completely, cancel solution inner canister and put on electric hot plate, rufous is slowly heated in 120 DEG C
Steam is waved to the greatest extent, and continues to be concentrated into 2~3ml, is let cool, plus 20% sulfuric acid solution 2ml, 5% liquor potassic permanganate 0.5ml, is shaken up,
5% hydroxylamine hydrochloride solution to aubergine is added dropwise just to disappear, is transferred in 10ml measuring bottles, wash container with water, washing lotion is incorporated in measuring bottle
In, and scale is diluted to, and shake up, it is centrifuged if necessary, supernatant is taken, obtain final product.With method while reagent preparation blank solution.
Determination method is accurate to draw that blank solution is appropriate with need testing solution, the method under sighting target directrix curve preparation determine from
The content of mercury (Hg) in need testing solution is read on standard curve, is calculated, obtained final product.
Cupper determination (flame method)
Condition determination Detection wavelength is 324.7nm, using Air-acetylene Flame, background correction is carried out if necessary.
The preparation precision of copper Standard Reserving Solution measures copper single element standard liquid in right amount, is diluted with 2% salpeter solution, is made
Solution per 1ml cupric (Cu) 10 μ g, obtains final product (0~5 DEG C of storage).
Precision measures copper Standard Reserving Solution in right amount respectively for the preparation of standard curve, and every 1ml difference is made of 2% salpeter solution
The μ g of cupric 0,0.05 μ g, 0.2 μ g, 0.4 μ g, 0.6 μ g, the solution of 0.8 μ g.Flame, mensuration absorbance, with absorbance are sprayed into successively
It is ordinate, concentration is abscissa, draws standard curve.
The preparation of need testing solution determines the preparation of need testing solution under item with lead.
Determination method is accurate to draw blank solution with need testing solution in right amount, and the method under the preparation of sighting target directrix curve is surveyed
It is fixed.The content of copper (Cu) from need testing solution is read on standard curve, calculates, and obtains final product.
Result judgement：This product is leaded must not cross 5mg/kg, cadmium must not cross 0.3mg/kg, arsenic must not cross 2mg/kg, mercury must not
Crossing 0.2mg/kg, copper must not cross 20mg/kg.
Organic chlorine agriculture chemicals residual quantity
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, Rotary Evaporators, supersonic wave cleaning machine, gas phase color
Spectrometer
Reagent and test solution：Petroleum ether (60~90 DEG C), acetone, sodium chloride, dichloromethane, anhydrous sodium sulfate (its petrochina
(60~90 DEG C) of ether is chromatographically pure, and other reagents are pure using analysis, and experimental water is purified water)
Reference substance：α-BHC, β-BHC, γ-BHC, δ δ-BHC, p, p '-DDE, p, p '-DDD, o, p '-DDT, p, p '-DDT,
PCNB agricultural chemical reference substances
Method：Determined according to persticide residue determination method (method of general rule 0,512 first).
Chromatographic condition is with system suitability with (14%- cyanogen propvl-phenvl) methyl polysiloxane or (5% phenyl) first
Based polysiloxane is the fused-silica capillary column (30m × 0.32mm × 0.25 μm) of fixer, the capture inspection of 63Ni-ECD electronics
Survey device.230 DEG C of injector temperature, 300 DEG C of detector temperature, Splitless injecting samples.Temperature programming：Initial 100 DEG C, 10 DEG C per minute
220 DEG C are risen to, 8 DEG C per minute rise to 250 DEG C, are kept for 10 minutes.Number of theoretical plate is calculated by α-BHC peaks and should be not less than 1 × 106,
The separating degree of two adjacent chromatographic peaks should be greater than 1.5.
The preparation precision of reference substance stock solution weighs BHC (BHC) (α-BHC, β-BHC, γ-BHC, δ-BHC), drop
DDT (DDT) (p, p '-DDE, p, p '-DDD, o, p '-DDT, p, p '-DDT) and pentachloronitrobenzene (PCNB) agricultural chemical reference substance are suitable
Amount, solution of every 1ml containing about 4~5 μ g is respectively prepared with petroleum ether (60~90 DEG C), is obtained final product.
The preparation precision for mixing reference substance stock solution measures above-mentioned each reference substance stock solution 0.5ml, in putting 10ml measuring bottles,
Scale is diluted to petroleum ether (60~90 DEG C), is shaken up, obtained final product.
The preparation precision of mixed reference substance solution measures above-mentioned mixing reference substance stock solution, with (60~90 DEG C) systems of petroleum ether
Contain the solution of 0 μ g, 1 μ g, 5 μ g, 10 μ g, 50 μ g, 100 μ g, 250 μ g respectively into every 1L, obtain final product.
The preparation of need testing solution takes test sample, is ground into powder (crossing No. three sieves), takes about 2g, accurately weighed, puts 100ml
In conical flask with cover, add water 20ml soaked overnights, and precision adds acetone 40ml, and weighed weight ultrasonically treated 30 minutes, lets cool, then
Weighed weight, supplies the weight of less loss with acetone, then adds sodium chloride about 6g, and precision adds methylene chloride 30ml, weighed weight, ultrasound
15 minutes, then weighed weight, the weight of less loss is supplied with dichloromethane, stand (making layering), organic phase is moved into rapidly and is equipped with
In the 100ml conical flask with cover of appropriate anhydrous sodium sulfate, place 4 hours.Precision measures 35ml, in concentrated under reduced pressure in 40 DEG C of water-baths
To near dry, plus a small amount of petroleum ether (60~90 DEG C) as it is preceding operate repeatedly it is cleared to dichloromethane and acetone, with petroleum ether (60~90
DEG C) dissolve and be transferred in 10ml tool plug graduated centrifuge tubes, plus petroleum ether (60~90 DEG C) precision is diluted to 5ml, is carefully added into
Sulfuric acid lml, shakes 1 minute, centrifugation (3000 revs/min) 10 minutes, and precision measures supernatant 2ml, puts the concentrate bottle of tool scale
In, rotary evaporator is connected, be concentrated into solution in right amount by (or using nitrogen) at 40 DEG C, and precision is diluted to 1ml, obtains final product.
Determination method is accurate respectively to be drawn need testing solution and corresponds each 1 μ l of mixed reference substance solution of concentration, note
Enter gas chromatograph, by 9 kinds of Residual Levels of Organochlorine Pesticides in external standard method calculating test sample.
Result judgement：This product (α-BHC, β-BHC, γ-BHC, δ-BHC sums) containing total BHC must not cross 0.2mg/kg,
Must not cross 0.2mg/kg, pentachloronitrobenzene must not mistake for total DDT (pp '-DDE, pp '-DDD, op '-DDT, pp '-DDT sums)
0.1mg/kg。
Water-soluble extractives
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, thermostat water bath, electric heating constant-temperature blowing drying box
Reagent and test solution：Water (reagent is pure using analysis, and experimental water is purified water)
Method is determined according to the cold-maceration under water-soluble extractives determination method (general rule 2201) item
Test sample about 4g is taken, accurately weighed, in putting the conical flask of 250~300ml, precision adds water 100ml, close plug, cold soaking,
Constantly shaken in first 6 hours, then stand 18 hours, filtered rapidly with filter is dried, precision measures subsequent filtrate 20ml, puts and has dried
Into the evaporating dish of constant weight, after being evaporated in water-bath, in 105 DEG C of dryings 3 hours, put and cool down 30 minutes in drier, rapid essence
Close weighed weight.Unless otherwise specified, the content (%) of water-soluble extractives in test sample is calculated with dry product.
Result judgement：This product water-soluble extractives must not be less than 17.0%.
AFB1
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, homogeneous bottle, centrifuge, high performance liquid chromatograph (are matched somebody with somebody
Put fluorescence detector and derivatization pump, derivatization incubator)
Reagent and test solution：(wherein acetonitrile is chromatographically pure, and other reagents are for methyl alcohol, acetonitrile, iodine, sodium chloride, immune affinity column
Analysis is pure, and experimental water is purified water)
Reference substance：AFB1Reference substance
Method：Determined according to aflatoxin determination method (general rule 2351).
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methanol-acetonitrile-water (40:
18: 42) be mobile phase；Detected using post-column derivation method, iodine derivatization method：Derivative solution be 0.05% iodine solution (take iodine 0.5g,
Adding methyl alcohol 100ml makes dissolving, is diluted with water to 1000ml and is made), derivatization flow rate pump 0.3ml per minute, derivatization temperature
70 DEG C are detected with fluorescence detector, excitation wavelength lambdaex=360nm (or 365nm), emission wavelength lambdaex=450nm.Two adjacent colors
The separating degree of spectral peak should be greater than 1.5.
The preparation precision of mixed reference substance solution measures AFB1(sign concentration is 1.0 μ g/ to reference substance solution
Ml) 0.5ml, in putting 10ml measuring bottles, with methanol dilution to scale, as stock solution.Precision measures stock solution 1ml, puts
In 25ml measuring bottles, with methanol dilution to scale, obtain final product.
The preparation of need testing solution takes test sample powder about 15g (crossing No. two sieves), accurately weighed, is placed in homogeneous bottle, plus
Enter sodium chloride 3g, precision adds 70% methanol solution 75ml, 2 minutes (mixing speed is more than 11000 revs/min) of high-speed stirred,
5 minutes (2500 revs/min of centrifugal speed) of centrifugation, precision measures supernatant 15ml, puts in 50ml measuring bottles, is diluted with water to quarter
Degree, shakes up, and with (0.45 μm) filtration of miillpore filter, measures subsequent filtrate 20.0ml, by immune affinity column, flow velocity 3ml per minute,
Eluted with water 20ml, eluent is discarded, and admits air into pillar, water is extruded into pillar, then eluted with proper amount of methanol, collect wash-out
Liquid, in putting 2ml measuring bottles, and with methanol dilution to scale, shakes up, and obtains final product.
Determination method is accurate respectively to draw the above-mentioned μ l of mixed reference substance solution 5,10 μ l, 15 μ l, 20 μ l, 25 μ l, injects liquid phase
Chromatograph, determines peak area, and with peak area as ordinate, sample size is abscissa, draws standard curve.Another accurate absorption is above-mentioned
The μ l of need testing solution 20~25, inject liquid chromatograph, determine peak area, equivalent to Huang from test sample is read on standard curve
Aspertoxin B1Amount, calculate, obtain final product.
Result judgement：This product contains AFB per 1000g15 μ g must not be crossed.
Sulfur dioxide residual quantity
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, electric jacket
Reagent and test solution：Hydrogen peroxide, methyl red ethanol solution, 0.01mol/L sodium hydroxide titrations liquid, hydrochloric acid solution
(6mol/L) (reagent is pure using analysis, and experimental water is purified water)
Method：Determined according to sulfur dioxide residual quantity determination method (general rule 2331).
Get it filled material or medicine materical crude slice fine powder about 10g, accurately weighed, puts in two neck round-bottom flasks, and add water 300~400ml.Open back
Stream condenser pipe switch feedwater, 100ml conical flasks bottom is placed in by a rubber wireway is connected at upper end E mouthfuls of condenser pipe.Taper
3% hydrogenperoxide steam generator 50ml is added in bottle as absorbing liquid (end of rubber wireway should be below absorbing liquid liquid level).Make
With preceding, 3 are added to drip methyl red ethanol solution indicator (2.5mg/ml) in absorbing liquid, and dripped with 0.01mol/L NaOH
Determine liquid and be titrated to yellow (i.e. terminal；If it exceeds terminal, then should give up the absorbent solution).Nitrogen is opened, is adjusted using flowmeter
Throttle body flow is to about 0.2L/min；The piston of separatory funnel C is opened, hydrochloric acid solution (6mol/L) 10ml is flowed into cucurbit,
The solution in two neck flasks is immediately heated to boiling, and keeps micro-boiling；Boiling water in flask stops heating after 1.5 hours.Inhale
After receipts liquid lets cool, it is placed on magnetic stirring apparatus and is stirred continuously, titrated with sodium hydroxide titration liquid (0.01mol/L), is held to yellow
The continuous 20 seconds time is not taken off, and the result of titration is corrected with blank assay.
Result judgement：This product sulfur dioxide residual quantity must not cross 150mg/kg.
Assay
Astragaloside IV
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, apparatus,Soxhlet's, thermostat water bath, efficient liquid phase
Chromatograph
Reagent and test solution：Methyl alcohol, acetonitrile, water-saturated n-butanol, ammonia solution, D101 types macroporous absorbent resin, ethanol are (wherein
Acetonitrile is chromatographically pure, and other reagents are pure using analysis, and experimental water is purified water)
Reference substance：Astragaloside IV reference substance
Method：Determined according to high performance liquid chromatography (general rule 0512).
Chromatographic condition is tried with octadecylsilane chemically bonded silica as filler with system suitability；With acetonitrile-water (32: 68)
It is mobile phase；EISD is detected.Number of theoretical plate is calculated by Astragaloside IV peak and should be not less than 4000.
The preparation of reference substance solution takes Astragaloside IV reference substance in right amount, accurately weighed, plus methyl alcohol is made every 1ml containing 0.5mg
Solution, obtain final product.
The preparation of need testing solution takes powder about 4g in this product, accurately weighed, in putting apparatus,Soxhlet's, plus methyl alcohol 40ml, it is cold
Dipped night, then add methyl alcohol appropriate, it is heated to reflux 4 hours, extract solution recycling design is simultaneously concentrated to dryness, residue adds water 10ml, low-grade fever
Make dissolving, shaken with water saturated n-butanol and extracted 4 times, each 40ml merges n-butanol liquid, is fully washed with ammonia solution 2 times,
Each 40ml, discards ammoniacal liquor, and n-butanol liquid is evaporated, and the residue 5ml that adds water makes dissolving, lets cool, by D101 type macroporous absorbent resins
Post (internal diameter is 1.5cm, and pillar height is 12cm), is eluted with water 50ml, discards aqueous, then is eluted with 40% ethanol 30ml, is discarded and is washed
De- liquid, elutes after with 70% ethanol 80ml, collects eluent, is evaporated, and residue adds methyl alcohol to dissolve, and is transferred in 5ml measuring bottles, plus first
Alcohol shakes up to scale, obtains final product.
Determination method is accurate respectively to draw the μ l of reference substance solution 10,20 μ l, the μ l of need testing solution 20, injects liquid chromatograph,
Determine, calculated with external standard two-point method logarithmic equation, obtain final product.
Result judgement：This product is calculated by dry product, containing Astragaloside IV (C41H68O14) 0.044% must not be less than.
Calycosin glucoside
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, thermostat water bath, high performance liquid chromatograph
Reagent and test solution：(wherein acetonitrile is chromatographically pure, and other reagents are pure using analysis, experiment for methyl alcohol, acetonitrile, formic acid
It is purified water with water)
Reference substance：Calycosin glucoside reference substance
Method：Determined according to high performance liquid chromatography (general rule 0512).
Chromatographic condition is tried with octadecylsilane chemically bonded silica as filler with system suitability；With acetonitrile as mobile phase A,
It is Mobile phase B with 0.2% formic acid solution, the regulation according to the form below carries out gradient elution；Detection wavelength is 260nm.Number of theoretical plate
Being calculated by calycosin glucoside peak should be not less than 3000.
The preparation of reference substance solution takes calycosin glucoside reference substance in right amount, accurately weighed, plus methyl alcohol is made often
Solution of the 1ml containing 50ug, obtains final product.
The preparation of need testing solution takes this product powder (crossing No. four sieves) about 1g, accurately weighed, puts in round-bottomed flask, and precision adds
Enter methyl alcohol 50ml, weighed weight is heated to reflux 4 hours, lets cool, then weighed weight, and the weight of less loss is supplied with methyl alcohol, is shaken up,
Filtration, precision measures subsequent filtrate 25ml, and to doing, residue adds methyl alcohol to dissolve to recycling design, is transferred in 5ml measuring bottles, plus methyl alcohol is extremely
Scale, shakes up, and obtains final product.
Determination method is not accurate to draw reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, determines, i.e.,
.
Result judgement：This product is calculated by dry product, (the C of glucoside containing calycosin22H22O10) must not be less than
0.022%.
Microbial limit
Detection of Salmonella takes this product 10g, with the pancreas junket soybean of aseptic inoculation to appropriate volume (tested through method applicability and determined)
In peptone fluid nutrient medium, mix, by non-sterile product limit test of microbe：Control bacteria examination method is checked.
Result judgement：Detection of Salmonella must not be detected (10g).
Bile tolerance gram-negative bacteria takes this product, with aseptic pancreas junket soya peptone fluid nutrient medium as diluent, is made 1: 10
Test liquid, mixes, by non-sterile product limit test of microbe：Control bacteria examination method is checked.
Result judgement：Bile tolerance gram-negative bacteria should be less than 104cfu(1g)。
Claims (3)
1. the quality standard of the Radix Astragali qualitative, quantitative prepared slices of Chinese crude drugs, it is characterised in that：In current edition《Chinese Pharmacopoeia》Quality standard
On the basis of increase medicine bits impurity, AFB1, sulfur dioxide residual quantity, and improve the mark of Astragaloside IV in assay
Quasi- limit is improved to 0.044% from 0.040%, the standard limits of calycosin glucoside from 0.020% improve to
0.022%.
2. the quality standard of the Radix Astragali qualitative, quantitative prepared slices of Chinese crude drugs as described in claim 1, it is characterised in that：
Medicine bits impurity according to determination of foreign matter method (《Chinese Pharmacopoeia》Four general rules 2301 of version in 2015) determine (《Chinese Pharmacopoeia》2015
Four general rules of version hereinafter referred to as general rule), 3% should be crossed.
AFB1 is determined according to aflatoxin determination method (general rule 2351), and this product must not cross 5 μ g/ containing AFB1
kg。
Sulfur dioxide residual quantity is determined according to sulfur dioxide residual quantity determination method (general rule 2331), and this product sulfur dioxide residual quantity must not
Cross 150mg/kg.
3. the manufacturing process of the Radix Astragali qualitative, quantitative prepared slices of Chinese crude drugs, it is characterised in that prepare the Radix Astragali Chinese medicine drink of 0.3~1mm of slice thickness
Piece, comprises the following steps：
A10 net systems：The impurity that is mixed in the Radix Astragali of removing and the product that go mouldy etc., or the Radix Astragali is carried out into stepping by size, it is clean to reach
It is net or be processed further treatment.Note：The Radix Astragali must not directly contact ground after cleaning.
A20 demulcens：The Radix Astragali after net system is put into medicine processing device, demulcen 20min-1h under vacuum negative pressure condition, is thoroughly moistened to the Radix Astragali
Thoroughly, plane of rupture is without the dry heart.Demulcen parameter：55-60 DEG C of temperature, pressure -0.05MPa, spray time 1s, spray time delay 100s.Note
Meaning：The Radix Astragali need to run through, and plane of rupture is soft or hard suitable inside and outside the Radix Astragali without the dry heart.
A30 cuttings：Piece 0.3~1mm of thickness, is operated by fully automatic high-speed slicer operational procedure, mixes up knife away from the Radix Astragali is tried
Cut, detected with slide measure, adjust cutting thickness, formally cut medicine after meeting the requirements again.
A40 is dried：It is dried using heated-air circulation oven, Radix Astragali material is laid on baking oven shelf, paving thickness is uniform, thickness
In below 3cm.Switch is opened, heater switch, blower fan is opened, 50 ± 2 DEG C are dried in temperature, and design temperature is reached in temperature
After dry 3-4h, drying is finished, and closes heater switch, continues to dry, and treats that the temperature inside the box is fallen to 35~40 DEG C, closes blower fan.
Post personnel need to fill in intermediate products and please examine list after drying, hand over Quality Mgmt Dept to carry out moisture inspection by QA samplings.
A50 is packed：Packed according to the requirement of this product packing specification.Need to check make-up room before packaging, confirm packaging life
Clearing out a gathering place for producing line has been completed, and checks whether packaging material meet the requirements.Inner packing：Being adjusted in equipment needs printing
Date of manufacture, lot number, QA monitoring, the Radix Astragali for weighing predetermined weight are put into hopper, are sealed with sealing machine, it is desirable to accomplish that sealing is tight
It is close, smooth, attractive in appearance.External packing：Adjusted in equipment the date of manufacture and lot number that need to be printed, QA monitoring, in external packing cases
Upper printing lot number, date of manufacture, should be noted whether lot number and date of manufacture are clear in print procedure.By the drink after the completion of inner packing
Piece and survey report are put into outsourcing box, 4 bags/box.Every 10 box medicine materical crude slice is inserted in 1 heat shrinkage film, carries out thermal contraction；Heat
It is fitted into after contraction in big carton, 240 boxes/case.In operating process, QA is inspected by random samples at any time.Post personnel need to fill in finished product and ask after packaging
Inspection is single, hands over Quality Mgmt Dept to carry out product examination by QA samplings.
A60, finished product：Post personnel need to fill in finished product and please examine list after packaging, hand over Quality Mgmt Dept to carry out product examination by QA samplings.
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| CN107823252A (en) * | 2017-11-23 | 2018-03-23 | 甘肃惠森药业发展有限公司 | A kind of processing method for improving astragaloside content |
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| CN110367363A (en) * | 2019-08-28 | 2019-10-25 | 甘肃国丽康中药材研发有限责任公司 | Radix Astragali bubble boils dedicated medicine materical crude slice and preparation method thereof |
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| CN108815219A (en) * | 2018-07-17 | 2018-11-16 | 广州今典精方药业有限公司 | A kind of tubers qualitative, quantitative prepared slices of Chinese crude drugs |
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| CN110367363A (en) * | 2019-08-28 | 2019-10-25 | 甘肃国丽康中药材研发有限责任公司 | Radix Astragali bubble boils dedicated medicine materical crude slice and preparation method thereof |
| CN110833571A (en) * | 2019-12-13 | 2020-02-25 | 宁夏隆德县六盘山中药资源开发有限公司 | Preparation method of astragalus membranaceus decoction piece finished product |
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