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Method for identifying andrographolide in lotus kernel antiphlogistic dropping pill

A technology of andrographolide, dropping pills, applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of identification interference, unclear spots, inability to meet identification requirements, etc., and achieves the effect of clear spots and easy observation.

Inactive Publication Date: 2017-05-17
天长亿帆制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After 3 batches of sample tests, the test product showed spots of the same color at the corresponding positions of the dehydroandrographolide reference substance, but no spots or spots were not clear at the corresponding positions of the andrographolide reference substance, which could not meet the requirements for identification. Interference of Polyethylene Glycol in Danxiaoyan Dropping Pills on Identification of Andrographolide

Method used

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  • Method for identifying andrographolide in lotus kernel antiphlogistic dropping pill
  • Method for identifying andrographolide in lotus kernel antiphlogistic dropping pill

Examples

Experimental program
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Effect test

Embodiment 1

[0021] This embodiment is a thin-layer identification experiment carried out according to the prior art method (Appendix VIB of Chinese Pharmacopoeia 2005 edition), and the specific process is as follows:

[0022] Take an appropriate amount of Liandan Xiaoyan Dropping Pills, grind it into a fine powder, accurately weigh 1g of the fine powder with a weighing balance, add 10ml of ethanol, soak for 20 minutes, ultrasonicate for 10 minutes, filter, and the filtrate is used as the test solution. Take andrographolide reference substance and dehydroandrographolide reference substance, respectively add ethanol to make a solution containing 1mg per 1ml, as the reference substance solution. Take 5 μl of each of the above three solutions, spot them on the same silica gel G thin-layer plate, use chloroform-methanol (9.5:0.5) as the developer, develop, take out, dry in the air, and spray with 10% phosphomolybdic acid ethanol solution , heated at 105°C until the spots were clearly colored. ...

Embodiment 2

[0024] Take an appropriate amount of Liandan Xiaoyan Dropping Pills, grind it into a fine powder, accurately weigh 1g of the fine powder with a weighing balance, add 15ml of purified water, ultrasonicate for 10 minutes, add water-saturated ethyl acetate, shake and extract twice, each 10ml each time, combine the extracts, evaporate to dryness, add 1ml methanol to the residue to dissolve as the test solution; take the andrographolide reference substance and the dehydroandrographolide reference substance, add ethanol respectively to make a solution containing 1mg per 1ml, as a contrast product solution. Take 2 μl of each of the above three solutions, spot them on the same silica gel GF254 thin-layer plate, use chloroform-ethyl acetate-methanol (20:15:2) as the developing agent, develop, take out, dry in the air, and place under ultraviolet light ( 254nm). Test results: in the chromatogram of the test product, on the position corresponding to the chromatogram of the andrographoli...

Embodiment 3

[0026] It is basically the same as Example 2, except that the extraction solvent is water-saturated butyl acetate, and the volume ratio of chloroform-ethyl acetate-methanol is 18:13:1.5. Test results and figure 2 same.

[0027] Example 3

[0028] It is basically the same as Example 2, except that the extraction solvent is propyl acetate, and the volume ratio of chloroform-ethyl acetate-methanol is 21:16:2.4. Test results and figure 2 same.

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Abstract

The invention provides a method for identifying andrographolide in a lotus kernel antiphlogistic dropping pill. The method comprises the following steps: 1) taking the lotus kernel antiphlogistic dropping pill as a raw material, grinding the lotus kernel antiphlogistic dropping pill, adding purified water and ultrasonically treating, taking acetate or C4-C6 alcohol as an extracting solvent for extracting, drying an extracting solution, and adding methyl alcohol into the residue and dissolving, thereby acquiring a tested solution; 2) respectively taking an andrographolide reference substance and a dehydrated andrographolide reference substance, and respectively adding into ethyl alcohol and preparing into solutions, thereby acquiring the reference solutions; and 3) taking trichloromethane-ethyl acetate-methyl alcohol as a developing solvent, respectively sucking and dropping the tested solution, the andrographolide reference solution and the dehydrated andrographolide reference solution on a same silica gel GF254 thin plate, unfolding, taking out, drying and viewing in 254nm wavelength. According to the identifying method, the interference of polyethylene glycol in the lotus kernel antiphlogistic dropping pill to the andrographolide is eliminated and the definition of the andrographolide in chromatography is increased.

Description

technical field [0001] The invention belongs to the technical field of drug detection, and in particular relates to a method for identifying andrographolide in Liandan Xiaoyan dripping pills. Background technique [0002] Liandan Xiaoyan Dropping Pills is a traditional Chinese medicine preparation, the medicinal materials are Andrographis paniculata and bitter wood, and the excipients are polyethylene glycol 4000, polyethylene glycol 6000 and liquid paraffin. Its effect is to clear away heat and detoxify, cool blood and reduce swelling. Fever, sore throat, sore mouth and tongue, sudden cough and overworked cough, hot dripping and astringent pain. [0003] Liandan Xiaoyan Dropping Pills are currently in compliance with the State Food and Drug Administration standard YBZ05602009. The method for identifying andrographolide and dehydroandrographolide in this standard is: take an appropriate amount of this product, grind it finely, take 1g, add 10ml of ethanol, soak for 20 minut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/90
CPCG01N30/90
Inventor 薛礼运周文艳范石虎刘晓玲牛鹏森马汉林
Owner 天长亿帆制药有限公司
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