CN102836323A - Preparation method of Zhidai tablets - Google Patents
Preparation method of Zhidai tablets Download PDFInfo
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- CN102836323A CN102836323A CN2012103570737A CN201210357073A CN102836323A CN 102836323 A CN102836323 A CN 102836323A CN 2012103570737 A CN2012103570737 A CN 2012103570737A CN 201210357073 A CN201210357073 A CN 201210357073A CN 102836323 A CN102836323 A CN 102836323A
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Abstract
The invention provides a preparation method of Zhidai tablets. The Zhidai tablets are prepared by taking 195g of diversifolious patrinia root, 195g of radix sophorae flavescentis, 260g of cherokee rose fruit, 130g of salt-fried common anemarrhena rhizome and 130g of fried atractylodes rhizome as active pharmaceutical ingredients and carrying out supercritical extraction and microwave extraction. By adopting the preparation method, the content of matrine is greatly increased.
Description
Technical field
The present invention relates to the Chinese medicine preparation technical field, be specifically related to a kind of method for preparing of controlling strap.
Background technology
Control strap and be recorded in Ministry of Public Health standard WS3-B-0102-89, process as crude drug, ability eliminating damp-heat, leukorrhagia stopping by Radix Patriniae heterophyllae 195g, Radix Sophorae Flavescentis 195g, Fructus Rosae Laevigatae 260g, Rhizoma Anemarrhenae (parched with salt) 130g, Rhizoma Atractylodis (parched) 130g.Be used for damp invasion of lower energizer, leucorrhea with bloody discharge, leucorrhea, fulminant leucorrhagia with yellowish discharge.
In the prior art, Shang Weiyou controls strap and is extracting the report that adopts supercritical and microwave technology aspect the preparation, and the method that powder and decocting boil is beaten in employing; Technology is coarse, backward, and impurity is many, causes patient's consumption excessive; Be inconvenient to take, had a strong impact on these article and used clinically.
Summary of the invention
Goal of the invention:, the object of the present invention is to provide a kind of method for preparing of controlling strap in order to address the above problem.
Technical scheme: the objective of the invention is to realize through following scheme:
A kind of method for preparing of controlling strap is processed as crude drug by Radix Patriniae heterophyllae 195g, Radix Sophorae Flavescentis 195g, Fructus Rosae Laevigatae 260g, Rhizoma Anemarrhenae (parched with salt) 130g, Rhizoma Atractylodis (parched) 130g, and described method is made up of the following step: get Rhizoma Atractylodis (parched), join CO
2In the supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 4-6%, extracting pressure 15-30MPa, temperature 30-50 ℃, CO
2Flow 1-3m1/g crude drug min, extraction time 150-180min gets supercritical extract, and is subsequent use; Get Radix Patriniae heterophyllae, Radix Sophorae Flavescentis, Fructus Rosae Laevigatae, Rhizoma Anemarrhenae (parched with salt), pulverize, add 70% ethanol of 2L, drop in the microwave extracting apparatus and carry out microwave extracting; Extraction power 400-600W extracts 2 times, and each 4-8 minute, combining extraction liquid; Concentrate, be added on the D101 macroporous adsorptive resins, 50% ethanol elution is collected 5 times of amount column volume eluents; Decompression recycling ethanol concentrates and drying, gets the microwave extraction thing, and is subsequent use; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol system granule, drying, tabletting is processed 1000, every heavy 0.5g.
Above-mentioned a kind of method for preparing of controlling strap, said CO
2The percent by volume that the supercritical extraction entrainer accounts for total extractant is 5%.
Above-mentioned a kind of method for preparing of controlling strap, said microwave extracting power 500W extracted 6 minutes at every turn.
Above-mentioned a kind of method for preparing of controlling strap, said CO
2The extracting pressure 20MPa of supercritical extraction, 40 ℃ of temperature, CO
2Flow 2ml/g crude drug min, extraction time 160min.
In the prior art, control every 0.5g of strap, each 5-8 sheet, 2-3 time on the one, that adopts that the present invention is prepared into controls every 0.5g of strap, and 4 of need were only taken 2-3 time on the 1st at every turn, had significantly reduced dose having under the condition of more active component.This conclusion can be through following evidence.
The comparison of controlling matrine content in the strap of test one, distinct methods preparation
1, instrument and reagent the present invention control strap: press the preparation of embodiment 3 methods, use the 910g crude drug, process 1000 through extracting, every heavy 0.5g.The former strap of controlling by the preparation of ministry standard method, uses the 910g crude drug, processes 1000 through extracting, every heavy 0.5g.Agilent 1200 high performance liquid chromatographs; METTLER AE240 electronic analytical balance; Matrine reference substance (Nat'l Pharmaceutical & Biological Products Control Institute).
2, method
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; Methanol-water-phosphoric acid (40:60:0.2) is a mobile phase; The detection wavelength is 280nm.Number of theoretical plate is pressed the matrine peak and is calculated, and should be not less than 3000.
The preparation of reference substance solution: precision takes by weighing at 4 hours matrine reference substance of 60 ℃ of drying under reduced pressure an amount of, adds methanol and processes the solution that every 1ml contains 18 μ g, promptly gets.
The preparation of need testing solution: get the present invention and control strap and the former strap of controlling, porphyrize, mixing is got 1g, and accurate the title, decide, the accurate 70% ethanol 20ml that adds, close plug, supersound process 10 minutes, centrifugal, get supernatant, promptly get.
Accurate respectively reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, and promptly get.
3, result
The result shows, the present invention controls that content of matrine is the 4.13mg/ sheet in the strap; And formerly control that content of matrine is the 1.33mg/ sheet in the strap, under the situation that dose reduces, matrine content improves a lot.
Above-mentioned research shows, adopts the strap of controlling of the present invention's preparation, and active constituent content is higher than the strap of controlling of ministry standard method preparation.
The specific embodiment
Below through the embodiment form; Foregoing of the present invention is remake further detailed description; But should this be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following instance, all technology that realizes based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
Get Radix Patriniae heterophyllae 195g, Radix Sophorae Flavescentis 195g, Fructus Rosae Laevigatae 260g, Rhizoma Anemarrhenae (parched with salt) 130g, Rhizoma Atractylodis (parched) 130g,, join CO Rhizoma Atractylodis (parched)
2In the supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 4%, extracting pressure 15MPa, 30 ℃ of temperature, CO
2Flow 1m1/g crude drug min, extraction time 150min gets supercritical extract, and is subsequent use; Get Radix Patriniae heterophyllae, Radix Sophorae Flavescentis, Fructus Rosae Laevigatae, Rhizoma Anemarrhenae (parched with salt), pulverize, add 70% ethanol of 2L, drop in the microwave extracting apparatus and carry out microwave extracting; Extraction power 400W extracts 2 times, and each 4 minutes, combining extraction liquid; Concentrate, be added on the D101 macroporous adsorptive resins, 50% ethanol elution is collected 5 times of amount column volume eluents; Decompression recycling ethanol concentrates and drying, gets the microwave extraction thing, and is subsequent use; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol system granule, drying, tabletting is processed 1000, every heavy 0.5g.
Through detecting, content of matrine is the 4.01mg/ sheet in the finished product.
Embodiment 2
Get Radix Patriniae heterophyllae 195g, Radix Sophorae Flavescentis 195g, Fructus Rosae Laevigatae 260g, Rhizoma Anemarrhenae (parched with salt) 130g, Rhizoma Atractylodis (parched) 130g,, join CO Rhizoma Atractylodis (parched)
2In the supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 6%, extracting pressure 30MPa, 50 ℃ of temperature, CO
2Flow 3m1/g crude drug min, extraction time 180min gets supercritical extract, and is subsequent use; Get Radix Patriniae heterophyllae, Radix Sophorae Flavescentis, Fructus Rosae Laevigatae, Rhizoma Anemarrhenae (parched with salt), pulverize, add 70% ethanol of 2L, drop in the microwave extracting apparatus and carry out microwave extracting; Extraction power 600W extracts 2 times, and each 8 minutes, combining extraction liquid; Concentrate, be added on the D101 macroporous adsorptive resins, 50% ethanol elution is collected 5 times of amount column volume eluents; Decompression recycling ethanol concentrates and drying, gets the microwave extraction thing, and is subsequent use; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol system granule, drying, tabletting is processed 1000, every heavy 0.5g.
Through detecting, content of matrine is the 3.97mg/ sheet in the finished product.
Embodiment 3
Get Radix Patriniae heterophyllae 195g, Radix Sophorae Flavescentis 195g, Fructus Rosae Laevigatae 260g, Rhizoma Anemarrhenae (parched with salt) 130g, Rhizoma Atractylodis (parched) 130g,, join CO Rhizoma Atractylodis (parched)
2In the supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 5%, extracting pressure 20MPa, 40 ℃ of temperature, CO
2Flow 2m1/g crude drug min, extraction time 160min gets supercritical extract, and is subsequent use; Get Radix Patriniae heterophyllae, Radix Sophorae Flavescentis, Fructus Rosae Laevigatae, Rhizoma Anemarrhenae (parched with salt), pulverize, add 70% ethanol of 2L, drop in the microwave extracting apparatus and carry out microwave extracting; Extraction power 500W extracts 2 times, and each 6 minutes, combining extraction liquid; Concentrate, be added on the D101 macroporous adsorptive resins, 50% ethanol elution is collected 5 times of amount column volume eluents; Decompression recycling ethanol concentrates and drying, gets the microwave extraction thing, and is subsequent use; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol system granule, drying, tabletting is processed 1000, every heavy 0.5g.
Through detecting, content of matrine is the 4.13mg/ sheet in the finished product.
Claims (4)
1. a method for preparing of controlling strap is processed as crude drug by Radix Patriniae heterophyllae 195g, Radix Sophorae Flavescentis 195g, Fructus Rosae Laevigatae 260g, Rhizoma Anemarrhenae (parched with salt) 130g, Rhizoma Atractylodis (parched) 130g, it is characterized in that described method is made up of the following step: get Rhizoma Atractylodis (parched), join CO
2In the supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 4-6%, extracting pressure 15-30MPa, temperature 30-50 ℃, CO
2Flow 1-3m1/g crude drug min, extraction time 150-180min gets supercritical extract, and is subsequent use; Get Radix Patriniae heterophyllae, Radix Sophorae Flavescentis, Fructus Rosae Laevigatae, Rhizoma Anemarrhenae (parched with salt), pulverize, add 70% ethanol of 2L, drop in the microwave extracting apparatus and carry out microwave extracting; Extraction power 400-600W extracts 2 times, and each 4-8 minute, combining extraction liquid; Concentrate, be added on the D101 macroporous adsorptive resins, 50% ethanol elution is collected 5 times of amount column volume eluents; Decompression recycling ethanol concentrates and drying, gets the microwave extraction thing, and is subsequent use; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol system granule, drying, tabletting is processed 1000, every heavy 0.5g.
2. according to the said a kind of method for preparing of controlling strap of claim 1, it is characterized in that said CO
2The percent by volume that the supercritical extraction entrainer accounts for total extractant is 5%.
3. according to the said a kind of method for preparing of controlling strap of claim 1, it is characterized in that said microwave extracting power 500W, extracted 6 minutes at every turn.
4. according to the said a kind of method for preparing of controlling strap of claim 1, it is characterized in that said CO
2The extracting pressure 20MPa of supercritical extraction, 40 ℃ of temperature, CO
2Flow 2ml/g crude drug min, extraction time 160min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103570737A CN102836323A (en) | 2012-09-22 | 2012-09-22 | Preparation method of Zhidai tablets |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103570737A CN102836323A (en) | 2012-09-22 | 2012-09-22 | Preparation method of Zhidai tablets |
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| CN102836323A true CN102836323A (en) | 2012-12-26 |
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| CN2012103570737A Pending CN102836323A (en) | 2012-09-22 | 2012-09-22 | Preparation method of Zhidai tablets |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103690755A (en) * | 2013-12-20 | 2014-04-02 | 青岛琴诚医药技术有限公司 | Application and preparation method of zhidai tablet |
| CN103784701A (en) * | 2014-03-05 | 2014-05-14 | 严白双 | Preparation method and application of leucorrhea treatment tablet |
-
2012
- 2012-09-22 CN CN2012103570737A patent/CN102836323A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103690755A (en) * | 2013-12-20 | 2014-04-02 | 青岛琴诚医药技术有限公司 | Application and preparation method of zhidai tablet |
| CN103690755B (en) * | 2013-12-20 | 2015-12-02 | 顾祥茂 | A kind of application controlling strap |
| CN103784701A (en) * | 2014-03-05 | 2014-05-14 | 严白双 | Preparation method and application of leucorrhea treatment tablet |
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Application publication date: 20121226 |