CN102836391A - Method for preparing compound salvia chinensis medicinal granule - Google Patents
Method for preparing compound salvia chinensis medicinal granule Download PDFInfo
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- CN102836391A CN102836391A CN2012103566182A CN201210356618A CN102836391A CN 102836391 A CN102836391 A CN 102836391A CN 2012103566182 A CN2012103566182 A CN 2012103566182A CN 201210356618 A CN201210356618 A CN 201210356618A CN 102836391 A CN102836391 A CN 102836391A
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Abstract
The invention provides a preparation method for preparing a compound salvia chinensis medicinal granule. The compound salvia chinensis medicinal granule is prepared by performing ultra-critical extraction and microwave extraction on 250g of salvia chinensis, 250g of red-rooted salvia root, 250g of suberect spatholobus stem, 150g of Chinese angelica, 150g of nutgrass galingale rhizome, 150g of turmeric root-tuber, 100g of safflower and 150g of turtle shell serving as bulk pharmaceuticals, so that the tanshinone content is increased greatly.
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 compound Zishen electuary.
Background technology
The compound Zishen electuary is recorded in Ministry of Public Health standard WS3-B-0113-89; Process as crude drug by Herba Salviae Chinensis 250g, Radix Salviae Miltiorrhizae 250g, Caulis Spatholobi 250g, Radix Angelicae Sinensis 150g, Rhizoma Cyperi 150g, Radix Curcumae 150g, Flos Carthami 100g, Carapax Trionycis 150g; The ability liver-smoothing, qi-regulating, blood circulation promoting and dispersing pathogen accumulation.Be used for the hepatosplenomegaly that advanced schistosomiasis causes.
In the prior art, the compound Zishen electuary is not arranged as yet at the report that adopts supercritical and microwave technology aspect the extraction preparation, and the method that adopts water to carry; 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 compound Zishen electuary 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 compound Zishen electuary; Process as crude drug by Herba Salviae Chinensis 250g, Radix Salviae Miltiorrhizae 250g, Caulis Spatholobi 250g, Radix Angelicae Sinensis 150g, Rhizoma Cyperi 150g, Radix Curcumae 150g, Flos Carthami 100g, Carapax Trionycis 150g; Described method is made up of the following step: get Radix Angelicae Sinensis, Rhizoma Cyperi, Radix Curcumae, Flos Carthami, 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 Herba Salviae Chinensis, Radix Salviae Miltiorrhizae, Caulis Spatholobi, Carapax Trionycis, 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 is processed 30 bags, every bag heavy 10g.
The method for preparing of above-mentioned a kind of compound Zishen electuary, said CO
2The percent by volume that the supercritical extraction entrainer accounts for total extractant is 5%.
The method for preparing of above-mentioned a kind of compound Zishen electuary, said microwave extracting power 500W extracted 6 minutes at every turn.
The method for preparing of above-mentioned a kind of compound Zishen electuary 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.
In the prior art, every bag of 22g of compound Zishen electuary, each 1 bag, 3 times on the one, the every bag of 10g of compound Zishen electuary that adopts the present invention to be prepared into only needs 1 bag at every turn, takes 3 times in 1st, has significantly reduced dose having under the condition of more active component.This conclusion can be through following evidence.
The comparison of TANSHINONES content in the compound Zishen electuary of test one, distinct methods preparation
1, instrument and reagent compound Zishen electuary of the present invention: press the preparation of embodiment 3 methods, use the 1450g crude drug, process 30 bags through extracting, every bag heavy 10g, every bag contains the crude drug amount is 48.3g.Former compound Zishen electuary by the preparation of ministry standard method, uses the 1450g crude drug, processes 30 bags through extracting, every bag heavy 22g, and every bag contains the crude drug amount is 48.3g.Agilent 1200 high performance liquid chromatographs; The METTLERAE240 electronic analytical balance; TANSHINONES 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 TANSHINONES peak and is calculated, and should be not less than 3000.
The preparation of reference substance solution: precision takes by weighing at 4 hours TANSHINONES 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 compound Zishen electuary of the present invention and former compound Zishen electuary, 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 that the content of TANSHINONES is the 13.64mg/ bag in the compound Zishen electuary of the present invention; And the content of TANSHINONES is the 4.75mg/ bag in the former compound Zishen electuary, and under the situation that dose reduces, TANSHINONES content improves a lot.
Above-mentioned research shows, adopts the compound Zishen electuary of the present invention's preparation, and active constituent content is higher than the compound Zishen electuary 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 Herba Salviae Chinensis 250g, Radix Salviae Miltiorrhizae 250g, Caulis Spatholobi 250g, Radix Angelicae Sinensis 150g, Rhizoma Cyperi 150g, Radix Curcumae 150g, Flos Carthami 100g, Carapax Trionycis 150g,, join CO Radix Angelicae Sinensis, Rhizoma Cyperi, Radix Curcumae, Flos Carthami
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 Herba Salviae Chinensis, Radix Salviae Miltiorrhizae, Caulis Spatholobi, Carapax Trionycis, 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 is processed 30 bags, every bag heavy 10g, every bag contains the crude drug amount is 48.3g.
Through detecting, the content of TANSHINONES is the 12.83mg/ bag in the finished product.
Embodiment 2
Get Herba Salviae Chinensis 250g, Radix Salviae Miltiorrhizae 250g, Caulis Spatholobi 250g, Radix Angelicae Sinensis 150g, Rhizoma Cyperi 150g, Radix Curcumae 150g, Flos Carthami 100g, Carapax Trionycis 150g,, join CO Radix Angelicae Sinensis, Rhizoma Cyperi, Radix Curcumae, Flos Carthami
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 Herba Salviae Chinensis, Radix Salviae Miltiorrhizae, Caulis Spatholobi, Carapax Trionycis, 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 is processed 30 bags, every bag heavy 10g, every bag contains the crude drug amount is 48.3g.
Through detecting, the content of TANSHINONES is the 12.39mg/ bag in the finished product.
Embodiment 3
Get Herba Salviae Chinensis 250g, Radix Salviae Miltiorrhizae 250g, Caulis Spatholobi 250g, Radix Angelicae Sinensis 150g, Rhizoma Cyperi 150g, Radix Curcumae 150g, Flos Carthami 100g, Carapax Trionycis 150g,, join CO Radix Angelicae Sinensis, Rhizoma Cyperi, Radix Curcumae, Flos Carthami
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 Herba Salviae Chinensis, Radix Salviae Miltiorrhizae, Caulis Spatholobi, Carapax Trionycis, 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 is processed 30 bags, every bag heavy 10g, every bag contains the crude drug amount is 48.3g.
Through detecting, the content of TANSHINONES is the 13.64mg/ bag in the finished product.
Claims (4)
1. the method for preparing of a compound Zishen electuary; Process as crude drug by Herba Salviae Chinensis 250g, Radix Salviae Miltiorrhizae 250g, Caulis Spatholobi 250g, Radix Angelicae Sinensis 150g, Rhizoma Cyperi 150g, Radix Curcumae 150g, Flos Carthami 100g, Carapax Trionycis 150g; It is characterized in that described method is made up of the following step: get Radix Angelicae Sinensis, Rhizoma Cyperi, Radix Curcumae, Flos Carthami, 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 Herba Salviae Chinensis, Radix Salviae Miltiorrhizae, Caulis Spatholobi, Carapax Trionycis, 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 is processed 30 bags, every bag heavy 10g.
2. according to the method for preparing of the said a kind of compound Zishen electuary 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 method for preparing of the said a kind of compound Zishen electuary of claim 1, it is characterized in that said microwave extracting power 500W, extracted 6 minutes at every turn.
4. according to the method for preparing of the said a kind of compound Zishen electuary 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 |
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| CN2012103566182A CN102836391A (en) | 2012-09-22 | 2012-09-22 | Method for preparing compound salvia chinensis medicinal granule |
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| CN2012103566182A CN102836391A (en) | 2012-09-22 | 2012-09-22 | Method for preparing compound salvia chinensis medicinal granule |
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| CN102836391A true CN102836391A (en) | 2012-12-26 |
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| CN2012103566182A Pending CN102836391A (en) | 2012-09-22 | 2012-09-22 | Method for preparing compound salvia chinensis medicinal granule |
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Application publication date: 20121226 |