CN103463567B - Vinegar rhizoma curcumae decoction piece and processing method thereof - Google Patents
Vinegar rhizoma curcumae decoction piece and processing method thereof Download PDFInfo
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Abstract
The invention provides a vinegar rhizoma curcumae decoction piece. The decoction piece comprises more than 1% of curcumin and more than 0.9ml/100g of volatile oil. The invention further provides a processing method of the decoction piece. According to the processing method provided by the invention, the content of the curcumin in rhizoma curcumae can be improved effectively; the loss amount of the volatile oil is low under the specific processing condition, and the good preparation process is provided for vinegar-processed rhizoma curcumae.
Description
Technical field
The present invention relates to stir-baked RHIIZOMA CURCUMAE with vinegar decoction pieces and concocting method thereof.
Background technology
Rhizoma Curcumae, for monocotyledon Zingiberaceae Zingiberaceae Rhizoma Curcumae Curcuma phaeocaulisVal., or the dry rhizome of RADIX CURCUMAE (also known as Curcuma wenyujin) C.wenyujin Y.H.Chen et C.Ling, Guangxi zedoary (also known as C. kwangsinensis) C.kwangsiensis S.lee et C.F.Liang.Acrid in the mouth, hardship, warm in nature, return liver, spleen channel, can removing blood stasis promoting the circulation of QI to relieve pain, blood stasis dispelling.
The raw Rhizoma Curcumae property of medicine is suddenly high, and have the fraud of consumption impairment of QI blood, ferritic valetudinarian, invalid should not use, and its quality is hard in addition, is unfavorable for adjusting, and concocts so just pay attention to it from Lei Gong's Treatise on Preparation and Broiling of Materia Medica.The Rhizoma Curcumae of ancient Chinese medicine doctor Clinical practice is concocted kind and is mainly contained raw Rhizoma Curcumae, fries Rhizoma Curcumae, stir-baked RHIIZOMA CURCUMAE with vinegar, stewing Rhizoma Curcumae, wine Rhizoma Curcumae, oily Rhizoma Curcumae, Fructus Crotonis Rhizoma Curcumae (processed) etc.But that uses till today mostly is Rhizoma Curcumae, stir-baked RHIIZOMA CURCUMAE with vinegar and wine Rhizoma Curcumae, and wherein stir-baked RHIIZOMA CURCUMAE with vinegar decoction pieces is the most conventional, research is recorded comparatively detailed, and is recorded as Rhizoma Curcumae concocts kind by Pharmacopoeia of the People's Republic of China version one in 2010.
But Rhizoma Curcumae quality is solid, reaches and boil to the saturating heart, the technological parameter that control vinegar boils is difficult point is also key point.The concocting method that in " Chinese Pharmacopoeia " version in 2010, regulation Rhizoma Curcumae vinegar boils at present, its processing procedure parameter not clear and definite.
Summary of the invention
The object of the present invention is to provide a kind of stir-baked RHIIZOMA CURCUMAE with vinegar decoction pieces and concocting method thereof.
The invention provides a kind of stir-baked RHIIZOMA CURCUMAE with vinegar decoction pieces, in this decoction pieces, curcumin content is more than 1%; Volatile oil content is at more than 0.9ml/100g.
Further, in described decoction pieces, curcumin content is 1.00-1.10%; Volatile oil content is 0.90-1.00ml/100g.
Present invention also offers the concocting method of stir-baked RHIIZOMA CURCUMAE with vinegar, it comprises following operating procedure:
Get Rhizoma Curcumae medical material, add the vinegar of medical material weight 20%v/w and the water of 3 times of weight, after infiltrating 3h, boil, be adjusted to slow fire and boil 1h, take out section, put in 120 DEG C of drying baker and smoke 30min, taking-up is dried, and obtains stir-baked RHIIZOMA CURCUMAE with vinegar decoction pieces.
Further, described vinegar is rice vinegar.
Further, described rice vinegar is 9 degree of rice vinegars.
Further, 3h is infiltrated.
Concocting method of the present invention, effectively can improve curcumin content in Rhizoma Curcumae, and under the present invention's specifically process of preparing Chinese medicine condition, loss of volatile oil amount is low, for Rhizoma Curcumae (processed with vinegar) provides a kind of better preparation technology.
Detailed description of the invention
The concocting method of embodiment 1 stir-baked RHIIZOMA CURCUMAE with vinegar decoction pieces
Get Rhizoma Curcumae decoction pieces, add the vinegar of decoction pieces weight 20%v/w and the water of 3 times of weight, after infiltrating 3h, put after boiling in container, be adjusted to slow fire and boil 1h, take out, cut into slices while hot, after putting 120 DEG C of baking 30min, then dry, obtain stir-baked RHIIZOMA CURCUMAE with vinegar decoction pieces.
The investigation of embodiment 2 concocting method
1. test apparatus and material
1.1 instrument
Agilent1200 high performance liquid chromatograph (Agilent company of the U.S.)
Mettler AE240 100,000/electronic analytical balance (German Mettler company)
FA1104 ten thousand/electronic analytical balance (Shanghai balance equipment factory)
BP211D electronic analytical balance (German Sai Duolisi)
KQ-500E type medical supersonic washer (Kunshan ultrasonic instrument company limited)
Digital display thermostat water bath HH-4 (Guo Hua Electrical Appliances Co., Ltd)
Volatile oil extractor
PTHW common constant temperature electric heating cover 500ml, 1000ml(Henan Ai Bote Science and Technology Ltd.)
101A electric drying oven with forced convection (the sub-safe baking oven maker in Wujiang)
Evaporating dish
The micropore filter of 0.45 μm
1.2 material
Rhizoma Curcumae rhizome, is purchased from Sichuan lotus pond Chinese Medicinal Materials Markets (product batch number 20130625)
Curcumin reference substance, is purchased from Wei Keqi bio tech ltd of Sichuan Province (lot number: 201008, purity: HPLC >=98%);
Methanol is chromatographically pure, and water is distilled water (self-control), and other reagent is analytical pure
Table 1 processing aids table
2. test method and result
The qualification of 2.1 medical materials
Rhizoma Curcumae rhizome is purchased in double fluid Chongzhou City, Sichuan, according to pertinent regulations under " Chinese Pharmacopoeia " version in 2010 one 194 pages " Rhizoma Curcumae " items, tests, all meet the every regulation of standards of pharmacopoeia to purchased Rhizoma Curcumae.The investigation of 2.2 supplementary product kinds
2.2.1 concocting method
Take 7 parts, Rhizoma Curcumae rhizome, every part of 50g, add the yellow wine (8.0%vol) of 30%, white rice vinegar (3.5g/100mL), Rhizoma Zingiberis Recens Bulbus Allii aromatic vinegar (4g/100mL) respectively, secondary protects peaceful vinegar (4g/100mL), one-level protects peaceful vinegar (5g/100mL), superfine protect peaceful vinegar (6g/100mL), 9 degree of rice vinegars (9g/100mL) and appropriate water, be 100mL liquid to cumulative volume, infiltrate 3h, 70 ° of duration and degree of heating are boiled to vinegar liquid and are exhausted, without white core in decoction pieces, be placed in 120 ° of baking ovens and dry 30min, slightly dry again, obtain the processed product of Rhizoma Curcumae seven kinds of specifications, for subsequent use.
Pulverized No. two sieves, prepare curcumin reference substance and need testing solution measures each laboratory sample dried cream yield and curcumin content, according to comprehensive grading=dry cream content/dry cream maximum * 0.4+ curcumin content/curcumin maximum * 0.6, total score 100 points, calculate its comprehensive grading, scoring soprano is best processing aids.
2.2.2 the preparation of reference substance
Take curcumin reference substance appropriate, accurately weighed, put in 5mL volumetric flask, add methanol constant volume to scale, shake up, be mixed with 0.00049mgmL
-1solution, product solution, to obtain final product in contrast.
2.2.3 the preparation of test sample
The each 20g(of processed product powder taking Rhizoma Curcumae seven kinds of specifications respectively crosses No. two sieves), accurately weighed, add the ethanol of 8 times amount 80%, heating and refluxing extraction twice, each 1h, filters, merging filtrate, be settled to 320mL with the ethanol of 80%, draw 25mL, water-bath volatilizes, residue adds dissolve with methanol and is settled to 25mL, shake up, filter, to obtain final product.
2.2.4 dried cream yield measures
The each 20g(of processed product taking Rhizoma Curcumae seven kinds of specifications respectively crosses No. two sieves), accurately weighed, add the ethanol of 8 times amount 80%, heating and refluxing extraction twice, each 1h, filters, merging filtrate, is settled to 320mL with the ethanol of 80%, accurate absorption 50ml extracting solution, put into the evaporating dish being dried to constant weight, weight is set to M, and water-bath volatilizes, in 105 DEG C of baking ovens, drying 3 hours, takes out, then puts into the drying receptacle with vaseline sealing, cool after 30 minutes, weigh.Constant weight evaporating dish weight containing extracting solution is set to N, calculates the yield that gets dry extract as follows.Experimental result is in table 2.
2.2.5 curcumin assay chromatographic condition
Chromatographic column: Agilent1200 high performance liquid chromatograph (being furnished with automatic sampler, quaternary gradient pump, diode array detector, online degasser, Agilent Chem Station chromatographic work station, Agilent company of the U.S.)
Mobile phase: methanol: water (containing 5% glacial acetic acid)=75:25
Determined wavelength: 420nm
Column temperature: 25 °
Flow velocity: 1.0mL/min
2.2.6 methodological study
1. linear relationship is investigated
Accurate absorption concentration is 0.01mgmL respectively
-1curcumin reference substance solution 2,4,6,8,12, μ L sample introduction under above-mentioned chromatographic condition measures, repeat sample introduction, measure peak area value, with peak area meansigma methods for vertical coordinate, sample size is abscissa, drawing standard curve.Regression equation is Y=150000X-18418, r=0.9999.Result shows that curcumin is good linear relationship at 0.02 μ g ~ 0.12 μ g.
Table 2 curcumin reference substance peak area data
Result shows, linearly well.
2. precision test
Accurate absorption curcumin reference substance solution 10uL, continuous sample introduction 6 times, the results are shown in Table 3.
Table 3 Precision test result
Result shows, RSD<2%, and instrument precision is good.
3. stability test
Accurate draw stir-baked RHIIZOMA CURCUMAE with vinegar (9 degree of rice vinegars) need testing solution respectively at 0,2,4,6,8,12,18h sample introduction 10 μ L, measure its peak area, the results are shown in Table 4.
Table 4 stability test result
Result shows, RSD<2%, and sample is stable in 18h.
4. replica test
Parallel precision takes 6 parts of stir-baked RHIIZOMA CURCUMAE with vinegar powder (9 degree of rice vinegars) 1g, operates by under test sample item, obtained need testing solution, and sample introduction 10 μ L, the results are shown in Table 5 respectively.
Table 5 replica test result
Result shows, repeatability is good.
5. average recovery test
Accurately weighed 6 parts of stir-baked RHIIZOMA CURCUMAE with vinegar powder (9 degree of rice vinegars) 1g, puts in triangular pyramidal bottle, adds curcumin reference substance 0.0432mg(0.0072mg/ml reference substance solution 6mL respectively), by operating under test sample item and measuring by content assaying method, the results are shown in Table 6.
Table 6 average recovery result of the test
Result shows, the sample pipetting volume response rate is good.
From the experimental result of methodological study, every investigation result all meets the requirements, and the method is reproducible, and precision is high.
The investigation result of table 7 supplementary product kind
Result shows, the comprehensive grading of Rhizoma Zingiberis Recens Bulbus Allii aromatic vinegar is the highest, but considers there are other adjuvants such as Rhizoma Zingiberis Recens and Bulbus Allii in vinegar, therefore not as the investigation of this processing aids; The best adjuvant of 9 degree of rice vinegars needed for the Rhizoma Curcumae process of preparing Chinese medicine, the vinegar sold on the market is mainly distinguished with acidity difference, show that the concentration of vinegar is higher better as processing aids effect by this experimental result; In addition, also draw from this experiment, yellow wine is higher as Rhizoma Curcumae processing aids score, need further pharmacology further investigation.2.4 screening test
Take 9 parts of each 50g of Rhizoma Curcumae decoction pieces, according to following table experiment arrangement.
Table 8
| Tested number | Rice vinegar consumption/% | Decocting time/h | Water consumption/doubly | Infiltrating time/h |
| No. 1 | 20 | 1 | 3 | 1 |
| No. 2 | 20 | 1.5 | 6 | 3 |
| No. 3 | 20 | 2 | 9 | 5 |
| No. 4 | 30 | 1 | 6 | 5 |
| No. 5 | 30 | 1.5 | 9 | 1 |
| No. 6 | 30 | 2 | 3 | 3 |
| No. 7 | 40 | 1 | 9 | 3 |
| No. 8 | 40 | 1.5 | 3 | 5 |
| No. 9 | 40 | 2 | 6 | 1 |
By obtained 9 groups of stir-baked RHIIZOMA CURCUMAE with vinegar decoction pieces, be placed in 120 DEG C of baking ovens, dry, pulverized No. two sieves for subsequent use.
prepared by reference substance
Take curcumin reference substance appropriate, accurately weighed, put in 10mL volumetric flask, add methanol constant volume to scale, shake up, be mixed with 0.01mgmL
-1solution, product solution, to obtain final product in contrast.
prepared by test sample
Take vinegar Rhizoma Curcumae powder (crossing No. two sieves) each 20g respectively, accurately weighed, add the ethanol of 8 times amount 80%, heating and refluxing extraction twice, each 1h, filters, merging filtrate, be settled to 320mL with the ethanol of 80%, draw 25mL, water-bath volatilizes, residue adds dissolve with methanol and is settled to 25mL, shake up, filter, to obtain final product.
dried cream yield measures
9 groups of processed product test liquid 50ml in accurate absorption Rhizoma Curcumae table 8, put into the evaporating dish being dried to constant weight, weight is set to M, water-bath volatilizes, and in 105 DEG C of baking ovens, drying 3 hours, takes out, put into the drying receptacle with vaseline sealing again, cool after 30 minutes, weigh.Constant weight evaporating dish weight containing extracting solution is set to N, calculates the yield that gets dry extract as follows.
volatile oil content testing
With reference to " Chinese Pharmacopoeia " version annex XD determination of volatile oil Division A League Matches of French Football method in 2010, get 8 times of water gagings, reflux 6h.Read volatile oil scale.Volatile oil content=volatile oil volume/medical material amount * 100%
curcumin assay
Chromatographic condition is with 2.2
Table 99 groups of Rhizoma Curcumae vinegar product dried cream yield results
Table 10 9 groups of Rhizoma Curcumae vinegar product curcumin content
Table 11 9 groups of Rhizoma Curcumae vinegar product volatile oil contents
Measure each laboratory sample dried cream yield, curcumin content and volatile oil content, according to comprehensive grading=dry cream content/dry cream maximum * 0.3+ curcumin content/curcumin maximum * 0.35+ volatile oil content/volatile oil maximum * 0.35, calculate its comprehensive grading.Result of the test is in table 12.
Table 12 result of the test
Result shows: comprehensive practical operation, infiltrating time is too short may some large medical material vinegar immersion be moistened fewer, and the oversize production efficiency that affects of infiltrating time, therefore get intermediate value 3h, best processing procedure is: add 9 degree of rice vinegars and 3 times of water gagings of 20%, after infiltrating 3h, put after boiling in container and be adjusted to slow fire, boil 1h, take out, cut into slices while hot, slightly dry again after putting 120 DEG C of baking 30min, obtain stir-baked RHIIZOMA CURCUMAE with vinegar decoction pieces.
The confirmatory investigation of 2.5 best processing procedure
Table 13
After 9 degree of rice vinegars that the present invention adds medical material weight 20% are concocted Rhizoma Curcumae, effectively can remain with effective component content, achieve best process of preparing Chinese medicine effect, simultaneously, it is concocted effect and is also significantly better than 30%, 40% Rhizoma Curcumae (processed with vinegar), and this result shows, optimised process of the present invention is when using minimum rice vinegar, farthest remain effective ingredient, dramatically saves on cost of material.
Claims (1)
1. the concocting method of stir-baked RHIIZOMA CURCUMAE with vinegar, is characterized in that: it is concocted by following operating procedure:
Get Rhizoma Curcumae medical material, add the vinegar of medical material weight 20%v/w and the water of 3 times of weight, infiltrate 3h, boil, be adjusted to slow fire and boil 1h, take out section, put in 120 DEG C of drying baker and smoke 30min, taking-up is dried, and obtains stir-baked RHIIZOMA CURCUMAE with vinegar decoction pieces; Described vinegar is rice vinegar; Described rice vinegar is 9 degree of rice vinegars.
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| CN108186981B (en) * | 2018-01-27 | 2020-07-10 | 云南新世纪中药饮片有限公司 | A processing method of Curcumae rhizoma and its processed product |
| CN114146151A (en) * | 2018-09-11 | 2022-03-08 | 四川聚元药业集团有限公司 | Processing method of vinegar-processed curcuma zedoary and preparation method of vinegar-processed curcuma zedoary decoction pieces |
| CN113244354A (en) * | 2021-05-13 | 2021-08-13 | 河北国松堂制药有限公司 | Vinegar curcuma zedoary decoction pieces and processing method thereof |
| CN115403457B (en) * | 2022-08-16 | 2023-06-23 | 神威药业集团有限公司 | A method for preparing Curcuma rhizome extract |
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Effective date of registration: 20210728 Address after: 629000 No. 398, Longxing Road, economic and Technological Development Zone, Suining City, Sichuan Province Patentee after: Sichuan quantaitang traditional Chinese medicine decoction pieces Co.,Ltd. Address before: 611137 No. 1166, Willow Road, Wenjiang District, Sichuan, Chengdu Patentee before: Chengdu University of Traditional Chinese Medicine |