CN101524410A - Preparation method of corydalis tuber decoction pieces - Google Patents

Preparation method of corydalis tuber decoction pieces Download PDF

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Publication number
CN101524410A
CN101524410A CN200910097906A CN200910097906A CN101524410A CN 101524410 A CN101524410 A CN 101524410A CN 200910097906 A CN200910097906 A CN 200910097906A CN 200910097906 A CN200910097906 A CN 200910097906A CN 101524410 A CN101524410 A CN 101524410A
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decoction pieces
rhizoma corydalis
preparation
corydalis tuber
vinegar
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CN200910097906A
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袁珂
张虹
王麟
陈相涛
刘华亮
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Zhejiang A&F University ZAFU
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Zhejiang Forestry College
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Abstract

The invention discloses a preparation method of corydalis tuber decoction pieces, belonging to the technical field of traditional Chinese medicine. The method comprises: washing fresh corydalis tuber medicine materials to remove sand and mud, slicing the materials into pieces, adding rice vinegar to soak the materials through, spreading the materials for drying in shade, and then baking in an oven to obtain the corydalis tuber decoction pieces. The method features directly carrying out concocting preparation of the fresh corydalis tuber so as to simultaneously finish the field process and the concocting preparation process of the decoction pieces, thus omitting the heating step, reducing the loss of effective ingredients, and simplifying the technique, saving labor, time and energy; the effective ingredients dissolution rate and pharmacological effects of the processed corydalis tuber decoction pieces are both higher than those of the traditional vinegar broiling method, and the content of tetrahydropalmatine is higher than that of the traditional concocting method, thus improving the medicine effect.

Description

A kind of preparation method of Rhizoma Corydalis decoction pieces
Technical field
The invention belongs to technical field of Chinese medicines, be specifically related to a kind of preparation method of Rhizoma Corydalis decoction pieces.
Background technology
The act like a bully dry tuber of papaveraceae plant corydalis Corydalis yanhusuo W.T.Wang of unit, acrid in the mouth, hardship, temperature, return the liver spleen channel, invigorate blood circulation, circulation of qi promoting, pain relieving, have invigorate blood circulation, regulate the flow of vital energy, the effect of pain relieving, clinically be usually used in diseases such as chest pain, epigastric pain, amenorrhea dysmenorrhea, postpartum stagnation, treating swelling and pain by traumatic injury.Contain multiple alkaloid in the Rhizoma Corydalis, pharmacological evaluation proves that the Rhizoma Corydalis total alkaloids in the Rhizoma Corydalis, Rhizoma Corydalis first element, second element, ugly element all have stronger analgesic activity, and the analgesic activity with tetrahydropalmatine is the strongest especially.
The clinical processed product commonly used of Rhizoma Corydalis has living Rhizoma Corydalis, vinegar Rhizoma Corydalis.Vinegar system adopts processed with vinegar, vinegar to boil and steaming with vinegar more.Give birth to that the product tool is invigorated blood circulation, circulation of qi promoting, pain relieving effect; Strengthen the promoting the circulation of QI to relieve pain effect after the vinegar system." Chinese pharmacopoeia version in 2005 is recorded Rhizoma Corydalis concocting method make a living Rhizoma Corydalis and stir-baked RHIZOMA CORYDALIS with vinegar.Free alkaloid in the Rhizoma Corydalis is insoluble in water, the effect of vinegar system is the alkaloid that is insoluble in water to be combined with acetic acid generate acetate soluble in water, help the effective ingredient stripping, improve the decoction rate, heighten the effect of a treatment, strengthen analgesic activity, this also thinks that with tradition vinegar system goes into Liver Channel, strengthens its dispersing the depressed liver-QI for alleviating pain effect and matches.Therefore inherent composition stripping plays an important role adjuvant vinegar to processed product, so the prescription vinegar goods of using more.
Traditional method technology of Rhizoma Corydalis decoction pieces processing is loaded down with trivial details, and its step is to carry out processing in production place earlier, comprises links such as cleaning, boiling water boil, drying.Carry out the process of preparing Chinese medicine processing of decoction pieces then, comprise cleaning, drying,, links such as vinegar boils or steaming with vinegar or vinegar are fried, dry, cutting, drying.In the process of preparing Chinese medicine processing of processing in production place and decoction pieces dry link and heating process are arranged all, especially medical material will not only be wasted a large amount of time and the energy through twice an oven dry heating and a vinegar system heating, has also increased effective ingredient and has run off and destructive chance.We as the index composition, carry out assay to commercially available vinegar system Rhizoma Corydalis decoction pieces with tetrahydropalmatine, and the content of finding the effective ingredient tetrahydropalmatine is well below the pharmacopeia specified standard.And the Rhizoma Corydalis processing procedure fully by virtue of experience lacks scientific and reasonable technological parameter and quantized quality control index at present, is unfavorable for the control of prepared slice quality.
Summary of the invention
At above-mentioned situation, the purpose of this invention is to provide a kind of technical scheme of preparation method of the Rhizoma Corydalis decoction pieces that can improve tetrahydropalmatine content, and then increased content of effective in the Rhizoma Corydalis decoction pieces, play synergic effect.
The preparation method of described a kind of Rhizoma Corydalis decoction pieces, it is characterized in that may further comprise the steps: fresh Rhizoma Corydalis medical material is removed impurity, water is got earth express developed, cut into the thin slice that thickness is 2-6mm, add the moistening with rice vinegar 4-8h of 30-45%, spread out and dry in the shade, in being 40-70 ℃ baking oven, temperature dries by the fire 6-18h, take out, airing promptly gets the Rhizoma Corydalis decoction pieces to room temperature.
The preparation method of described a kind of Rhizoma Corydalis decoction pieces is characterized in that: the thickness of Rhizoma Corydalis medical material thin slice is 2-5mm.
The preparation method of described a kind of Rhizoma Corydalis decoction pieces is characterized in that: the thickness of Rhizoma Corydalis medical material thin slice is 3-4mm.
The preparation method of described a kind of Rhizoma Corydalis decoction pieces is characterized in that: the concentration of rice vinegar is 32-45%, preferred 35-40%.
The preparation method of described a kind of Rhizoma Corydalis decoction pieces is characterized in that: the moistening time is 3-7h, preferred 4-6h, more preferably 5-6h.
The preparation method of described a kind of Rhizoma Corydalis decoction pieces is characterized in that: oven temperature is 45-60 ℃, preferred 50-55 ℃.
The preparation method of described a kind of Rhizoma Corydalis decoction pieces is characterized in that: drying time is 9-16h, preferred 10-15h, more preferably 11-14h, most preferably 12-13h.
The preparation method of above-mentioned a kind of Rhizoma Corydalis decoction pieces, be that the bright product of Rhizoma Corydalis are directly concocted processing, owing to be that the process of preparing Chinese medicine course of processing of processing in production place and decoction pieces is finished simultaneously, boil with regard to having reduced the boiling water in the processing in production place like this, dry run and concoct dry and heating vinegar system process in early stage in the processing, only through cleaning, cutting, vinegar profit system, dry four steps, be heated link and loss of active ingredients have been reduced, simplified technology, saved manpower, the time and the energy, and concocting process have specifically can foundation technological parameter and method of quality control, Rhizoma Corydalis decoction pieces effective ingredient dissolution rate and pharmacological action that processing obtains all are higher than traditional stir-baking with vinegar, the content of tetrahydropalmatine exceeds 27~43% than traditional concocting method, plays synergic effect.
The percentage composition that relates in the present specification, except other had explanation, the percentage composition of liquid was a volume ratio, solid percentage composition is a weight ratio.
Description of drawings
Fig. 1 is the high-efficient liquid phase chromatogram of tetrahydropalmatine reference substance;
The high-efficient liquid phase chromatogram of tetrahydropalmatine in the Rhizoma Corydalis decoction pieces that Fig. 2 makes for the present invention;
Abscissa is represented retention time among Fig. 1, Fig. 2, and vertical coordinate is represented peak height.
The specific embodiment
Now in conjunction with specific embodiments, the invention will be further described.
Embodiment 1
Fresh Rhizoma Corydalis medical material is removed impurity, and water is got earth express developed, cuts into the thin slice that thickness is 4mm, adds 40% moistening with rice vinegar 6h, and spread out and dry in the shade, be dry 12h in 50 ℃ the baking oven in temperature, to take out, airing promptly gets the Rhizoma Corydalis decoction pieces to room temperature.
Embodiment 2
Fresh Rhizoma Corydalis medical material is removed impurity, and water is got earth express developed, cuts into the thin slice that thickness is 3mm, adds 30% moistening with rice vinegar 5h, and spread out and dry in the shade, be dry 10h in 60 ℃ the baking oven in temperature, to take out, airing promptly gets the Rhizoma Corydalis decoction pieces to room temperature.
Embodiment 3
Fresh Rhizoma Corydalis medical material is removed impurity, and water is got earth express developed, cuts into the thin slice that thickness is 4mm, adds 35% moistening with rice vinegar 4h, and spread out and dry in the shade, be dry 8h in 70 ℃ the baking oven in temperature, to take out, airing promptly gets the Rhizoma Corydalis decoction pieces to room temperature.
Below by corresponding test the preparation technology of above-mentioned Rhizoma Corydalis decoction pieces and the Rhizoma Corydalis decoction pieces that makes are carried out assay.
One, the Rhizoma Corydalis decoction pieces that makes is carried out assay:
Chromatographic condition and system suitability test: chromatographic column: Waters Xbridge ODSC 18(250mm * 4.6mm, 5 μ m); Mobile phase: methanol-0.1% phosphate aqueous solution (triethylamine adjust pH to 6.0) (55: 45); Detect wavelength: 280nm; 25 ℃ of column temperatures; Flow velocity: 1.0mLmin -125 ℃ of column temperatures.
The preparation of reference substance solution: tetrahydropalmatine reference substance 13.00mg decided in accurate title, place the 250mL measuring bottle, add dissolve with methanol and be diluted to scale, shake up, filter through 0.45 μ m microporous filter membrane, filtrate becomes the reference substance solution that every 1mL contains tetrahydropalmatine 0.052mg.
The preparation of need testing solution: take by weighing the same place of production by the Rhizoma Corydalis decoction pieces of traditional concocting method processing and each the about 5.00g of Rhizoma Corydalis decoction pieces that processes by embodiment 1, the accurate title, decide, in the flask, accurate strong ammonia solution-methanol (1: 20) mixed solution 500mL that adds claims to decide weight at the bottom of the horizontalization, 1 hour post-heating of merceration refluxed 1 hour, put coldly, claim again to decide weight, supply with strong ammonia solution-methanol (1: 20) mixed solution and subtract weight loss, shake up, filter accurate subsequent filtrate 25mL, the evaporate to dryness drawn, residue adds dissolve with methanol, be transferred in the 5mL measuring bottle, be diluted to scale, shake up with methanol, filter through 0.45 μ m microporous filter membrane, filtrate is as need testing solution.
Linear relationship is investigated: precision measure tetrahydropalmatine reference substance solution 2,, 5,10,20,40 μ L inject high performance liquid chromatograph respectively, measure by above-mentioned chromatographic condition.(μ g) is abscissa with the reference substance sample size, is vertical coordinate drawing standard curve with the peak area integrated value, and the regression equation that calculates tetrahydropalmatine is Y=8.02 * 10 5X+7.57 * 10 2, r=0.9999.The result shows that tetrahydropalmatine is good linear relationship with peak area in 0.104~2.08 μ g scope.
Precision is investigated: the accurate reference substance solution 20 μ L that draw, inject high performance liquid chromatograph, continuous sample introduction 6 times is measured the peak area integrated value respectively under above-mentioned chromatographic condition, the relative standard deviation RSD that calculates tetrahydropalmatine is 0.48%, shows that precision is good.
Repeatability is investigated: get 5 parts of same sample coarse powder, and every part of about 5.00g, the accurate title, decide, and presses the preparation of need testing solution preparation method.Get need testing solution 20 μ L, inject high performance liquid chromatograph, measure the peak area integrated value of tetrahydropalmatine under above-mentioned chromatographic condition, the relative standard deviation RSD that calculates tetrahydropalmatine is 2.05%.
Stability test: get same need testing solution 20 μ L respectively, in 2,4,8,10,12h injects high performance liquid chromatograph, measures the peak area integrated value of tetrahydropalmatine under above-mentioned chromatographic condition.The relative standard deviation RSD that calculates tetrahydropalmatine is 0.65%, and the result shows that need testing solution is stable in 12h.
The average recovery test: the Rhizoma Corydalis decoction pieces by traditional concocting method processing that takes by weighing known content reaches each the about 2.50g of Rhizoma Corydalis decoction pieces that processes by embodiment 1, and precision claims fixed, and precision adding reference substance solution is an amount of, presses the preparation method preparation of above-mentioned need testing solution.Sample thief test liquid 20 μ L inject high performance liquid chromatograph, measure the peak area integrated value of tetrahydropalmatine under above-mentioned chromatographic condition, and the average recovery that calculates tetrahydropalmatine is 99.61%, and calculating relative standard deviation RSD is 0.98%.
Sample size is measured: take by weighing and break into coarse powder (crossing sieve No. 3) and by the Rhizoma Corydalis decoction pieces of traditional concocting method processing and press each 5 parts of the Rhizoma Corydalis decoction pieces of embodiment 1 processing, every part of about 0.5g accurately claims surely, and the preparation method of pressing above-mentioned need testing solution prepares.Get need testing solution 10 μ L, inject high performance liquid chromatograph, measure the peak area integrated value of tetrahydropalmatine.The result is 0.886mgg by the content of tetrahydropalmatine in the Rhizoma Corydalis decoction pieces of traditional concocting method processing -1, and be 1.263mgg by the content of tetrahydropalmatine in the Rhizoma Corydalis decoction pieces of embodiment 1 processing -1
Adopt said method that the Rhizoma Corydalis decoction pieces of embodiment 2, example 3 is carried out assay, the content of tetrahydropalmatine is respectively 1.126mgg in the Chinese medicine Rhizoma Corydalis decoction pieces as a result -1And 1.223mgg -1The content of tetrahydropalmatine exceeds 27~43% than traditional concocting method in the Rhizoma Corydalis decoction pieces of the present invention's preparation.
Two, the technological parameter of the preferred Rhizoma Corydalis decoction pieces of orthogonal experiment processing method
Content with tetrahydropalmatine serves as to investigate index, selects L for use 9(3 4) orthogonal scheme, with the medical material slice thickness, with vinegar amount and 3 factors of baking temperature, 3 levels of each factor design orthogonal test to optimize best processing procedure, the results are shown in Table 1, table 2, table 3.
Table 1 factor level table
Figure A20091009790600071
Table 2 Orthogonal experiment results
Figure A20091009790600081
Table 3 analysis of variance table
Figure A20091009790600082
Annotate: F 0.05(2,2)=19 F 0.01(2,2)=99
Interpretation of result: blank column D item R value is less, as error term.From the intuitive analysis of result of the test and variance analysis as can be seen, factor A, B and C have appreciable impact to experimental result, and factor A selects level 3, and promptly selecting slice thickness is 4mm; Factor B selects level 3, and promptly selecting with the vinegar amount is 40%; K 3c>K 2c>K 1c, factor C selects level 2, and promptly baking temperature is 50 ℃, so, determine that finally the optimised process that Rhizoma Corydalis is concocted is A 3B 3C 2, be about to Rhizoma Corydalis and at source take advantage of fresh slices 4mm thickness, after the drying, spray 40% rice vinegar, dry down at 50 ℃.
In above-mentioned preparation method: the thickness of Rhizoma Corydalis medical material thin slice is 2mm, 5mm, 6mm; The concentration of rice vinegar is 35%, 42%, 45%; The moistening time is 7h, 8h; Oven temperature is 40 ℃, 45 ℃, 55 ℃, 65 ℃; Drying time is 9h, 10h, 11h, 12h, 13h, 14h, 15h, 16h, 17h, 18h, and other condition is identical, and tetrahydropalmatine also can reach content of the present invention in the Rhizoma Corydalis decoction pieces that makes.

Claims (7)

1, a kind of preparation method of Rhizoma Corydalis decoction pieces, it is characterized in that may further comprise the steps: fresh Rhizoma Corydalis medical material is removed impurity, water is got earth express developed, cut into the thin slice that thickness is 2-6mm, add the moistening with rice vinegar 4-8h of 30-45%, spread out and dry in the shade, in being 40-70 ℃ baking oven, temperature dries by the fire 6-18h, take out, airing promptly gets the Rhizoma Corydalis decoction pieces to room temperature.
2, the preparation method of a kind of Rhizoma Corydalis decoction pieces as claimed in claim 1 is characterized in that: the thickness of Rhizoma Corydalis medical material thin slice is 2-5mm.
3, the preparation method of a kind of Rhizoma Corydalis decoction pieces as claimed in claim 1 is characterized in that: the thickness of Rhizoma Corydalis medical material thin slice is 3-4mm.
4, the preparation method of a kind of Rhizoma Corydalis decoction pieces as claimed in claim 1 is characterized in that: the concentration of rice vinegar is 32-45%, preferred 35-40%.
5, the preparation method of a kind of Rhizoma Corydalis decoction pieces as claimed in claim 1 is characterized in that: the moistening time is 3-7h, preferred 4-6h, more preferably 5-6h.
6, the preparation method of a kind of Rhizoma Corydalis decoction pieces as claimed in claim 1 is characterized in that: oven temperature is 45-60 ℃, preferred 50-55 ℃.
7, the preparation method of a kind of Rhizoma Corydalis decoction pieces as claimed in claim 1 is characterized in that: drying time is 9-16h, preferred 10-15h, more preferably 11-14h, most preferably 12-13h.
CN200910097906A 2009-04-23 2009-04-23 Preparation method of corydalis tuber decoction pieces Pending CN101524410A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102119968A (en) * 2011-01-26 2011-07-13 浙江省中药研究所有限公司 Method for processing and preparing fresh rhizoma corydalis
CN104906197A (en) * 2015-05-19 2015-09-16 亳州蜀中药业有限公司 Method for processing rhizoma corydalis decoction pieces
CN106706633A (en) * 2016-05-21 2017-05-24 广州今典精方药业有限公司 Quality standard and manufacturing process of corydalis tuber qualitative and quantitative traditional Chinese medicine decoction piece

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102119968A (en) * 2011-01-26 2011-07-13 浙江省中药研究所有限公司 Method for processing and preparing fresh rhizoma corydalis
CN102119968B (en) * 2011-01-26 2013-03-13 浙江省中药研究所有限公司 Method for processing and preparing fresh rhizoma corydalis
CN104906197A (en) * 2015-05-19 2015-09-16 亳州蜀中药业有限公司 Method for processing rhizoma corydalis decoction pieces
CN106706633A (en) * 2016-05-21 2017-05-24 广州今典精方药业有限公司 Quality standard and manufacturing process of corydalis tuber qualitative and quantitative traditional Chinese medicine decoction piece

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