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Method for determining content of lithospermum erythrorhizon and application

A measurement method and technology of comfrey, applied in the field of medical technology detection, can solve the problems of long measurement time, affecting the production progress of white etched pills, and high comprehensive cost, and achieve the effect of shortening the detection time, saving labor costs and instrument operating costs

Pending Publication Date: 2022-03-11
GUANGZHOU BAIYUNSHAN ZHONGYI PHARMA COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The determination process of β,β′-dimethylacryloylarkanin in Zicao can be simplified into four steps: sample pretreatment, preparation of reference solution, HPLC analysis, and data processing. The determination of the content of β′-dimethylacryloyl arcanin takes a long time, usually more than 19 hours, and the overall cost is relatively high. At the same time, the quality inspection of Zicao is also the longest time required for the quality inspection of all medicinal materials in Baishi Pills. Seriously affected the production schedule of white etching pills

Method used

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  • Method for determining content of lithospermum erythrorhizon and application
  • Method for determining content of lithospermum erythrorhizon and application
  • Method for determining content of lithospermum erythrorhizon and application

Examples

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Embodiment 1

[0050] The present embodiment provides a method for detecting the content of β, β′-dimethylacryloylarkanin in Comfrey, specifically as follows:

[0051] 1 Instrument and solution preparation

[0052] 1.1 Instrument

[0053] Column: Shiseido SPOLAR C 18 (250mm) column.

[0054]1.2 Preparation of reference substance solution: Take an appropriate amount of β,β′-dimethylacryloylarkanin reference substance, weigh it accurately, add acetonitrile-water-formic acid (70:30:0.05) solvent to prepare 0.1mg per 1mL solution, that is;

[0055] 1.3 Preparation of the test solution: Take about 0.5 g of the test comfrey powder (passed through a No. 4 sieve), weigh it accurately, put it in a stoppered conical flask, add 25 ml of petroleum ether (60-90°C) accurately, and weigh it. Determine the weight, sonicate for 30 minutes, let cool, weigh again, make up the lost weight with petroleum ether (60-90°C), shake well, and filter. Precisely measure 10ml of the subsequent filtrate, evaporate to...

Embodiment 2

[0062] The present embodiment provides a method for detecting the content of β, β′-dimethylacryloylarkanin in Comfrey, specifically as follows:

[0063] 1 Instrument and solution preparation

[0064] 1.1 Instrument

[0065] Column: Waters Xbridge C 18 (250mm) column.

[0066] 1.2 Preparation of reference substance solution: Take an appropriate amount of β,β′-dimethylacryloylarkanin reference substance, weigh it accurately, add acetonitrile-water-formic acid (70:30:0.05) solvent to prepare 0.1mg per 1mL solution, that is;

[0067] 1.3 Preparation of the test solution: Take about 0.5 g of the test comfrey powder (passed through a No. 4 sieve), weigh it accurately, put it in a stoppered conical flask, add 25 ml of petroleum ether (60-90°C) accurately, and weigh it. Determine the weight, sonicate for 30 minutes, let cool, weigh again, make up the lost weight with petroleum ether (60-90°C), shake well, and filter. Precisely measure 10ml of the subsequent filtrate, evaporate to...

Embodiment 3

[0074] The present embodiment provides a method for detecting the content of β, β′-dimethylacryloylarkanin in Comfrey, specifically as follows:

[0075] 1 Instrument and solution preparation

[0076] 1.1 Instrument

[0077] Column: Shiseido MGII C 18 (250mm) column.

[0078] 1.2 Preparation of reference substance solution: Take an appropriate amount of β,β′-dimethylacryloylarkanin reference substance, weigh it accurately, add acetonitrile-water-formic acid (70:30:0.05) solvent to prepare 0.1mg per 1mL solution, that is;

[0079] 1.3 Preparation of the test solution: Take about 0.5 g of the test comfrey powder (passed through a No. 4 sieve), weigh it accurately, put it in a stoppered conical flask, add 25 ml of petroleum ether (60-90°C) accurately, and weigh it. Determine the weight, sonicate for 30 minutes, let cool, weigh again, make up the lost weight with petroleum ether (60-90°C), shake well, and filter. Precisely measure 10ml of the subsequent filtrate, evaporate to ...

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Abstract

The invention provides a lithospermum content determination method which comprises the following steps: mixing beta, beta '-dimethylacryloyl alkannin with a first solvent to prepare a reference substance; the first solvent comprises a mixture of acetonitrile, water and formic acid; mixing radix arnebiae seu lithospermi with a second solvent, filtering, taking filtrate, evaporating to dryness, mixing with the first solvent, filtering, taking filtrate, and preparing a test sample; respectively performing high performance liquid chromatography determination on the test sample and the reference substance, wherein the conditions of high performance liquid chromatography determination are as follows: a mobile phase is a mixture of acetonitrile, water and formic acid in a volume ratio of (61-79): (21-39): 0.05; the column temperature is 25-35 DEG C; the flow velocity is 1.2 ml / min to 1.5 ml / min. According to the detection method, the required time is short and is only 8 hours, so that the comprehensive cost is saved to a great extent.

Description

technical field [0001] The invention relates to the field of medical technology detection, in particular to a content determination method and application of comfrey. Background technique [0002] Comfrey, also known as hard comfrey and soft comfrey, is a herbal medicine included in the Chinese Pharmacopoeia. It has a sweet, salty, cold nature, heart-guiding and liver meridian. It has the effects of cooling blood, detoxifying rashes, promoting blood circulation and removing blood stasis. Sheng, purple and black macules, opaque measles, sores, eczema, water and fire burns, etc. [0003] Content determination is one of the important inspection items of comfrey medicinal materials, and the quality of comfrey medicinal materials can be judged by determining the content of active components of comfrey. β,β′-Dimethacryloyl arcanin is one of the active ingredients in comfrey. The determination process of β,β′-dimethylacryloylarkanin in Zicao can be simplified into four steps: sam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/32G01N30/34
CPCG01N30/02G01N30/06G01N30/32G01N30/34G01N2030/324
Inventor 郑健茵黎炳华谢晓玲胡家敏邝永全麦洁雪袁洁丽周伟健
Owner GUANGZHOU BAIYUNSHAN ZHONGYI PHARMA COMPANY