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Method for quantitatively detecting polytypes of chrysophanol and emodin in rhubarb and compound preparation of rhubarb

A compound preparation and quantitative determination technology, which is applied in the direction of measuring devices, test sample preparation, instruments, etc., can solve the problems of coated impurity peaks, difficult to identify emodin, etc., achieve simple methods, save testing costs, and ensure accuracy Effect

Inactive Publication Date: 2009-12-16
韩桂茹
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  • Description
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Problems solved by technology

[0011] 2. Aiming at the problem of difficult-to-identify emodin-coated impurity peaks, through the reorganization and proportion discussion of mobile phase components, methanol- 0.1% phosphoric acid (85:15) is the mobile phase, which solves the difficult problem of difficult identification of emodin-coated impurity peaks (see figure 2 ), each peak is well separated, and is suitable for various reversed-phase chromatographic columns currently on the market, ensuring the accuracy of the measurement results

Method used

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  • Method for quantitatively detecting polytypes of chrysophanol and emodin in rhubarb and compound preparation of rhubarb
  • Method for quantitatively detecting polytypes of chrysophanol and emodin in rhubarb and compound preparation of rhubarb
  • Method for quantitatively detecting polytypes of chrysophanol and emodin in rhubarb and compound preparation of rhubarb

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example 1

[0064] Quantitative Determination of Rhubarb in Example 1 Dahuang Zhechong Pills

[0065] 【Content Determination】Determination according to high performance liquid chromatography (Appendix VI D of Chinese Pharmacopoeia I).

[0066] Chromatographic conditions and system suitability test Octadecylsilane bonded silica gel is used as filler; acetonitrile-methanol-0.1% phosphoric acid (40~45:20~27:38~30) is used as mobile phase; detection wavelength is 254nm. The number of theoretical plates should not be less than 3000 based on the chrysophanol peak.

[0067] Preparation of Reference Substance Solution Take appropriate amount of chrysophanol and emodin reference substance, weigh them accurately, add methanol to make a mixed solution containing 10 μg of chrysophanol and 5 μg of emodin per 1 ml, and obtain it.

[0068] Preparation of the test solution Take this product water honeyed pills, grind finely, take 0.5g, and accurately weigh; or take small honeyed pills or large honeyed p...

example 2

[0072] Example 2 Quantitative Determination of Rhubarb in Maren Runchang Pills

[0073] 【Content Determination】Determination according to high performance liquid chromatography (Appendix VI D of Chinese Pharmacopoeia I).

[0074] Chromatographic conditions and system suitability test Octadecylsilane bonded silica gel is used as filler; acetonitrile-methanol-0.1% phosphoric acid (40~45:20~27:38~30) is used as mobile phase; detection wavelength is 254nm. The number of theoretical plates should not be less than 3000 based on the chrysophanol peak.

[0075] Preparation of reference substance solution Accurately weigh chrysophanol and emodin reference substance, add methanol to make a mixed solution containing 10 μg of chrysophanol and 5 μg of emodin per 1 ml.

[0076] Preparation of the test solution Take the product under the weight difference item, cut it into pieces (less than 2mm in diameter), take 1g, weigh it accurately, put it in a stoppered Erlenmeyer flask, and accuratel...

example 3 6

[0080] Quantitative determination of rhubarb in Liuweian Xiaosan of example 3

[0081] 【Content Determination】Determination according to high performance liquid chromatography (Appendix VI D of Chinese Pharmacopoeia I).

[0082] Chromatographic conditions and system suitability test Octadecylsilane bonded silica gel is used as filler; acetonitrile-methanol-0.1% phosphoric acid (40~45:20~27:38~30) is used as mobile phase; detection wavelength is 254nm. The number of theoretical plates should not be less than 3000 based on the chrysophanol peak.

[0083] Preparation of Reference Substance Solution Take appropriate amount of chrysophanol and emodin reference substance, weigh them accurately, add methanol to make a mixed solution containing 18 μg of chrysophanol and 8 μg of emodin per 1 ml, and obtain it.

[0084] Preparation of the test solution Take 0.8g of this product, accurately weigh it, put it in a stoppered Erlenmeyer flask, accurately add 25ml of methanol-hydrochloric ac...

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Abstract

The invention relates to a method for quantitatively detecting polytypes of chrysophanol and emodin in rhubarb and a compound preparation of rhubarb. The method is characterized by integrating methyl extraction and acid hydrolysis into one step; eliminating steps of extraction by poisonous solvents such as trichloromethane and the like, drying by vaporization and the like; and reducing the pre-processing time from original 10 to 15 hours to 0.5 hour, along with high efficiency, low cost and little pollution. By studying components and ratios of the flowing phase, acetonitrile-methyl alcohol-0.1 percent phosphoric acid (the mixing ratio is n 40-45:20-27:38-30) replaces methyl alcohol-0.1 percent phosphoric acid (the mixing ratio is 85:15) as the flowing phase, the problem of difficultly in identifying coating impurity peaks of the emodin is solved and the correctness of the detection result is ensured. The chrysophanol and the emodin are taken as detection indexes, the same flowing phase is used, and the chrysophanol and the emodin in total, ionization and combined anthraqunione in the preparation are detected at the same. The method has the advantages of combining the detection indexes and the efficacy of the preparation for the first time, improving the scientificity and rationality of the quality control indexes, and being suitably used for various preparations containing the rhubarb, along with simpleness, quickness and accuracy.

Description

technical field [0001] The invention relates to a method for quantitative determination of chrysophanol and emodin in polytypes in rhubarb and its compound preparation. Background technique [0002] Rhubarb has the effects of purging heat and dredging intestines, cooling blood and detoxification, and removing blood stasis to stimulate menstruation. Used for excess heat and constipation, stagnant abdominal pain, dysentery, damp-heat jaundice, vomiting of blood heat, red eyes, swollen throat, abdominal pain in the intestine, carbuncle and furuncle, blood stasis, amenorrhea, injury from falls, external treatment of water and fire burns ; Upper gastrointestinal bleeding. It is a traditional Chinese medicinal material with a large dosage and a high frequency of use in clinical practice. According to literature reports, rhubarb mainly contains rhubarb anthraquinones, which exist in polytypes such as free anthraquinone, combined anthraquinone and total anthraquinone. The represe...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N1/28
Inventor 韩桂茹王金龙赵志军冯丽封淑华
Owner 韩桂茹
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