CN101618060A - Method for controlling quality of euphorbia kansui decoction pieces - Google Patents
Method for controlling quality of euphorbia kansui decoction pieces Download PDFInfo
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- CN101618060A CN101618060A CN200810043590A CN200810043590A CN101618060A CN 101618060 A CN101618060 A CN 101618060A CN 200810043590 A CN200810043590 A CN 200810043590A CN 200810043590 A CN200810043590 A CN 200810043590A CN 101618060 A CN101618060 A CN 101618060A
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Abstract
The invention discloses a method for controlling quality of euphorbia kansui decoction pieces, which comprises a step of determining the content of 3-O-(2,3-dimethylbutanoyl)-13-O-oxododecyl ingenol and euphol in fresh and processed euphorbia kansui. The method uses the separated 3-O-(2,3-dimethylbutanoyl)-13-O-oxododecyl ingenol and euphol as indexes, establishes a method for detecting HPLC-ELSD for controlling the quality of the euphorbia kansui decoction pieces, has simple and quick operation, and is applicable to quality control of the fresh euphorbia kansui and the processed euphorbia kansui decoction pieces.
Description
Technical field
The present invention relates to a kind of method of quality control of Chinese medicine euphorbia kansui decoction pieces.
Background technology
The world today is under the influence of " going back to nature " ideological trend, the cry that natural drug is sought by many countries grows to even greater heights, and Chinese medicine has been subjected to the attention of countries in the world with its rich in natural resources, unique theoretical system, distinctive curative effect and lower characteristics such as toxic and side effects.But contain complicated composition in the Chinese medicine, be subjected to the influence of each side factor, difficult quality is stable, and most of Chinese medicine lacks strict quality method and quality standard, makes it to meet the requirement of international medical market, has seriously restricted the development of China's Chinese medicine industry.Therefore, Chinese medicine is combined with modern science and technology, set up practicable Chinese medicine quality control method and quality standard, realize that the modernization of Chinese medicine has become inexorable trend.
Radix Kansui is the dried root of euphorbia plant Radix Kansui Euphorbia kansui T.N.Liou ex T.P.Wang, main product in Shaanxi, ground such as Henan, Shandong, Gansu, Shanxi.Radix Kansui is cold in nature, and bitter in the mouth is poisonous, returns lung, kidney, large intestine channel, has the function of removing fluid-retention by purgation, is used for diseases such as cirrhotic ascites, hydrothorax, edema and difficulty in urination and defecation clinically more.Radix Kansui is toxic traditional Chinese medicine simply, and the product of giving birth to are only for external, for oral administration must the process of preparing Chinese medicine.So, at present in the living Radix Kansui of having of clinical practice and two kinds of specifications of Radix Kansui (processed).Chemical constituent is mainly naboom diterpene esters derivative and a small amount of triterpenoid compound in the Radix Kansui, also contains starch, Palmic acid, sucrose, citric acid, glucose, oxalic acid etc.The report of the composition Study aspect of relevant Radix Kansui is more, but is mostly chemical constituent is carried out the research of separation and purification aspect, does not see the research report of quality control aspect." quality control of euphorbia kansui decoction pieces is mainly differentiated by powder and the thin layer chromatography discriminating in the Chinese pharmacopoeia (version was an one in 2005), there are not index components or content of effective to measure, be difficult to like this guarantee the safe, effective of euphorbia kansui decoction pieces, also limited further research and development Radix Kansui.
Summary of the invention
At the above-mentioned deficiency of prior art, technical problem to be solved by this invention is to propose a kind ofly can effectively to control the euphorbia kansui decoction pieces method for quality.Use the inventive method and can carry out accurate quantitatively control euphorbia kansui decoction pieces.
Life of the present invention, Radix Kansui (processed) decoction pieces are according to " the disclosed method of Chinese pharmacopoeia (version was an one in 2005) is prepared from.
The present invention is an index to separate 3-O-(2,3-dimethyl butyrate the acyl group)-13-O-lauroyl ingenol and the euphadienol that obtain from life, Radix Kansui (processed) decoction pieces, and euphorbia kansui decoction pieces is carried out accurate quantitatively control.Formula I is the chemical structural formula of 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol, and formula II is the chemical structural formula of euphadienol.
Formula I
Formula II
Give birth to, the quality control of Radix Kansui (processed) decoction pieces at first is 3-O-(2 wherein; 3-dimethyl butyrate acyl group)-control of 13-O-lauroyl ingenol and euphadienol content; adopt high performance liquid chromatography to measure respectively to give birth to, the content of 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol and euphadienol in the Radix Kansui (processed) decoction pieces:
With the content of 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol in high effective liquid chromatography for measuring life, the Radix Kansui (processed) decoction pieces, chromatographic condition is to be filler with the octadecylsilane chemically bonded silica; Mobile phase is methanol-water, and gradient elution is (percentage ratio of time/methanol): 0～5 minute/70%～85%, 5～55 minutes/85%～95%; Detector is an evaporative light scattering detector, evaporating temperature: 110 ℃, and atomization temperature: 80 ℃, gas flow rate: 1.5L/min; Column temperature is 35 ℃; Sample size is 20 μ l; Flow velocity is 1.1ml/min; Theoretical cam curve is pressed 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol calculating should be not less than 10000;
With the content of euphadienol in high effective liquid chromatography for measuring life, the Radix Kansui (processed) decoction pieces, chromatographic condition is to be filler with the octadecylsilane chemically bonded silica; Mobile phase is methanol-water, and gradient elution is (percentage ratio of time/methanol): 0～10 minute/90%～100%; Detector is an evaporative light scattering detector, evaporating temperature: 110 ℃, and atomization temperature: 80 ℃, gas flow rate: 1.5L/min; Column temperature is 35 ℃; Sample size is 20 μ l; Flow velocity is 1.0ml/min; Theoretical cam curve is calculated by euphadienol should be not less than 10000.
Among the present invention, the content of giving birth to 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol in euphorbia kansui decoction pieces and the Radix Kansui (processed) decoction pieces must not be less than 0.23mg/g and 0.22mg/g; The content of giving birth to euphadienol in euphorbia kansui decoction pieces and the Radix Kansui (processed) decoction pieces must not be less than 1.22mg/g and 1.19mg/g.
The present invention is to separate the 3-O-(2 that obtains from life, Radix Kansui (processed) decoction pieces; 3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol and euphadienol are index; set up the HPLC-ELSD assay method of control euphorbia kansui decoction pieces quality, can carry out accurate quantitatively control life, Radix Kansui (processed) decoction pieces.The inventive method is easy and simple to handle, quick, is applicable to the quality control of living Radix Kansui and Radix Kansui (processed) decoction pieces.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.These embodiment are interpreted as only being used to the present invention is described and are not used in restriction protection scope of the present invention.After the content of having read the present invention's record, those skilled in the art can make various changes or modifications the present invention, and these equivalences change and modify and fall into claims of the present invention institute restricted portion equally.
Embodiment 1
(1) get 8 batches of living euphorbia kansui decoction pieces, be ground into fine powder, take by weighing about 2g available from Shanghai, Anhui, Sichuan, Hebei, Gansu, accurate claim fixed, add chloroform 10ml, ultrasonic twice, each 15 minutes, filter, merging filtrate, evaporate to dryness, residue add chloroform and are settled to 1ml, make need testing solution.Take by weighing 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol reference substance 5mg, the accurate title, decide, and adds dissolve with methanol and be settled to scale, makes the reference substance solution of 1.00mg/ml.Accurate above-mentioned reference substance solution and each 20 μ l of need testing solution of drawing, inject high performance liquid chromatograph respectively, with the octadecylsilane chemically bonded silica is filler, mobile phase is methanol-water, gradient elution is (percentage ratio of time/methanol): 0～5 minute/70%～85%, 5～55 minute/85%～95%, detector is an evaporative light scattering detector (evaporating temperature: 110 ℃, atomization temperature: 80 ℃, gas flow rate: 1.5L/min), column temperature is 35 ℃, and flow velocity is that 1.1ml/min measures and analyzes.
Testing result shows, the content range of 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol is 0.29-1.12mg/g in the 6 batches of living euphorbia kansui decoction pieces; And do not see in 2 batches of living euphorbia kansui decoction pieces available from Gansu and contain 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol.
(2) get 8 batches of living euphorbia kansui decoction pieces, be ground into fine powder, take by weighing about 1.2g available from Shanghai, Anhui, Sichuan, Hebei, Gansu, accurate claim fixed, add chloroform 5ml, ultrasonic twice, each 15 minutes, filter, merging filtrate, evaporate to dryness, residue add chloroform and are settled to 10ml, make need testing solution.Take by weighing euphadienol reference substance 5mg, the accurate title, decide, and adds dissolve with methanol and be settled to scale, obtains the reference substance solution of 0.50mg/ml.Accurate above-mentioned reference substance solution and each 20 μ l of need testing solution of drawing, inject high performance liquid chromatograph respectively, with the octadecylsilane chemically bonded silica is filler, mobile phase is methanol-water, and gradient elution is (percentage ratio of time/methanol): 0～10 minute/90%～100%, and detector is an evaporative light scattering detector (evaporating temperature: 110 ℃, atomization temperature: 80 ℃, gas flow rate: 1.5L/min), column temperature is 35 ℃, and flow velocity is that 1.0ml/min measures and analyzes.
Testing result shows, the content range of euphadienol is 1.52-4.70mg/g in the 6 batches of living euphorbia kansui decoction pieces; And do not see in 2 batches of living euphorbia kansui decoction pieces available from Gansu and contain euphadienol.
By the present embodiment decidable, be substandard product available from 2 batches of living euphorbia kansui decoction pieces in Gansu; All the other 6 batches of living euphorbia kansui decoction pieces available from Shanghai, Anhui, Sichuan and Hebei are qualified products.
Embodiment 2
(1) gets available from the homemade 10 batches of Radix Kansui (processed) decoction pieces of Shanghai, Anhui, Hebei and laboratory, press method mensuration 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol content wherein of embodiment 1 (1).As a result, the content range of 3-O-in 10 batches of Radix Kansui (processed) decoction pieces (2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol is 0.27-0.92mg/g.
(2) get available from the homemade 10 batches of Radix Kansui (processed) decoction pieces of Shanghai, Anhui, Hebei and laboratory, press the method mensuration euphadienol content wherein of embodiment 1 (2).As a result, the content range of euphadienol is 1.49-4.5mg/g in the 10 batches of Radix Kansui (processed) decoction pieces.
By the present embodiment decidable, be qualified products available from the homemade 10 batches of Radix Kansui (processed) decoction pieces of Shanghai, Anhui, Hebei and laboratory.
Claims (3)
1, a kind of method of quality control of euphorbia kansui decoction pieces is characterized in that: this method comprises 3-O-in life, the Radix Kansui (processed) decoction pieces (2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol and euphadienol Determination on content:
With the content of 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol in high effective liquid chromatography for measuring life, the Radix Kansui (processed) decoction pieces, chromatographic condition is to be filler with the octadecylsilane chemically bonded silica; Mobile phase is methanol-water, and gradient elution is: 0～5 minute/70%～85%, 5～55 minute/85%～95%; Detector is an evaporative light scattering detector, evaporating temperature: 110 ℃, and atomization temperature: 80 ℃, gas flow rate: 1.5L/min; Column temperature is 35 ℃; Sample size is 20 μ l; Flow velocity is 1.1ml/min; Theoretical cam curve is pressed 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol calculating should be not less than 10000;
With the content of euphadienol in high effective liquid chromatography for measuring life, the Radix Kansui (processed) decoction pieces, chromatographic condition is to be filler with the octadecylsilane chemically bonded silica; Mobile phase is methanol-water, and gradient elution is: 0～10 minute/90%～100%; Detector is an evaporative light scattering detector, evaporating temperature: 110 ℃, and atomization temperature: 80 ℃, gas flow rate: 1.5L/min; Column temperature is 35 ℃; Sample size is 20 μ l; Flow velocity is 1.0ml/min; Theoretical cam curve is calculated by euphadienol should be not less than 10000.
2, the method for quality control of euphorbia kansui decoction pieces according to claim 1 is characterized in that:
Method with 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol content in high effective liquid chromatography for measuring life, the Radix Kansui (processed) decoction pieces comprises the steps:
Euphorbia kansui decoction pieces is ground into fine powder, takes by weighing about 2g, accurate claim surely, add chloroform 10ml, ultrasonic twice, each 15 minutes, filter, merging filtrate, evaporate to dryness, residue add chloroform and are settled to 1ml, make need testing solution;
Take by weighing 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol reference substance 5mg, the accurate title, decide, and adds dissolve with methanol and be settled to scale, makes the reference substance solution of 1.00mg/ml;
Accurate above-mentioned reference substance solution and each 20 μ l of need testing solution of drawing inject high performance liquid chromatograph respectively, and the record chromatogram is pressed the content that peak area value calculates 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol in the euphorbia kansui decoction pieces;
Method with euphadienol content in high effective liquid chromatography for measuring life, the Radix Kansui (processed) decoction pieces comprises the steps:
Euphorbia kansui decoction pieces is ground into fine powder, takes by weighing about 1.2g, accurate claim surely, add chloroform 5ml, ultrasonic twice, each 15 minutes, filter, merging filtrate, evaporate to dryness, residue add chloroform and are settled to 10ml, make need testing solution;
Take by weighing euphadienol reference substance 5mg, the accurate title, decide, and adds dissolve with methanol and be settled to scale, makes the reference substance solution of 0.50mg/ml;
Accurate above-mentioned reference substance solution and each 20 μ l of need testing solution of drawing inject high performance liquid chromatograph respectively, and the record chromatogram is pressed the content that peak area value calculates euphadienol in the euphorbia kansui decoction pieces.
3, the method for quality control of euphorbia kansui decoction pieces according to claim 1 and 2, it is characterized in that: the content of giving birth to 3-O-(2,3-dimethyl butyrate acyl group)-13-O-lauroyl ingenol in euphorbia kansui decoction pieces and the Radix Kansui (processed) decoction pieces must not be less than 0.23mg/g and 0.22mg/g; The content of giving birth to euphadienol in euphorbia kansui decoction pieces and the Radix Kansui (processed) decoction pieces must not be less than 1.22mg/g and 1.19mg/g.
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| CN2008100435900A CN101618060B (en) | 2008-07-02 | 2008-07-02 | Method for controlling quality of euphorbia kansui decoction pieces |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214539A (en) * | 2013-05-08 | 2013-07-24 | 南京中医药大学 | Preparation method of euphol |
| CN106153840A (en) * | 2016-06-17 | 2016-11-23 | 中国中医科学院中药研究所 | A kind of tcm and herbal slice method for evaluating quality |
| CN109771469A (en) * | 2019-03-29 | 2019-05-21 | 张朔生 | A kind of vinegar toast root of gansui and its concocting method |
-
2008
- 2008-07-02 CN CN2008100435900A patent/CN101618060B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214539A (en) * | 2013-05-08 | 2013-07-24 | 南京中医药大学 | Preparation method of euphol |
| CN106153840A (en) * | 2016-06-17 | 2016-11-23 | 中国中医科学院中药研究所 | A kind of tcm and herbal slice method for evaluating quality |
| CN106153840B (en) * | 2016-06-17 | 2018-06-29 | 中国中医科学院中药研究所 | A kind of tcm and herbal slice method for evaluating quality |
| CN109771469A (en) * | 2019-03-29 | 2019-05-21 | 张朔生 | A kind of vinegar toast root of gansui and its concocting method |
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| CN101618060B (en) | 2011-05-25 |
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