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Method for measuring content of luteolin in lamiophlomis rotata pharmaceutical preparation by liquid chromatography

A pharmaceutical preparation and liquid chromatography technology, applied in the field of traditional Chinese medicine, can solve problems such as inaccurate determination of luteolin content, poor separation of luteolin peak and impurity peak, tailing phenomenon and the like

Active Publication Date: 2009-06-03
GANSU CHEEZHENG TIBETAN MEDICINE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the above system solution is used as the mobile phase, the separation of the luteolin peak and the impurity peak is poor, and there is a tailing phenomenon, which makes the content determination of luteolin not accurate enough

Method used

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  • Method for measuring content of luteolin in lamiophlomis rotata pharmaceutical preparation by liquid chromatography
  • Method for measuring content of luteolin in lamiophlomis rotata pharmaceutical preparation by liquid chromatography
  • Method for measuring content of luteolin in lamiophlomis rotata pharmaceutical preparation by liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Example 1: Determination of Luteolin Content in Tablets Containing Unique Medicinal Material

[0065] Determination according to high performance liquid chromatography (Appendix VID of "Chinese Pharmacopoeia" 2005 edition).

[0066] (1) Chromatographic conditions and system suitability test: use octadecylsilane bonded silica gel as filler (250mm×4.6mm, 5μm); use acetonitrile-tetrahydrofuran-mass concentration 0.5% phosphoric acid (20:6.4:73.6) as filler Mobile phase, column temperature 40°C; detection wavelength 350nm; flow rate 1.0ml / min; theoretical plate number according to luteolin (C 15 h 10 o 6 ) peak calculation should not be less than 5000.

[0067] (2) Preparation of reference substance solution: Accurately weigh 0.25 mg of luteolin reference substance dried with phosphorus pentoxide, put it in a volumetric bottle, add methanol to make a solution containing 5 μg per 1 ml, and obtain it.

[0068] (3) Preparation of the test solution: Take about 0.5g of this ...

Embodiment 2

[0070] Embodiment 2: Determination of luteolin content in plaster containing unique medicinal material

[0071] Determination according to high performance liquid chromatography (Appendix VID of "Chinese Pharmacopoeia" 2005 edition).

[0072] Steps (1), (2) are the same as in Example 1.

[0073] (3) Preparation of the test solution: take about 2 g of this product, accurately weigh it, accurately add 25 ml of 2.5 mol / L hydrochloric acid methanol solution (the volume ratio of hydrochloric acid to methanol is 2.25:10), weigh it, and heat to reflux for 30 Minutes, let cool, weighed again, supplemented the lost weight with methanolic hydrochloric acid solution, shaken up, filtered, accurately measured 2ml of the filtrate, put it in a measuring bottle, diluted it with methanol to 5ml, shaken up, and used 0.45 μm microporous membrane filtration, that is.

[0074] (4) Determination method: each 10 μ l of the reference substance solution and the test solution are accurately drawn, in...

Embodiment 3

[0075] Example 3: Determination of Luteolin Content in Pills Containing Unique Medicinal Material

[0076] Determination according to high performance liquid chromatography (Appendix VID of "Chinese Pharmacopoeia" 2005 edition).

[0077] Steps (1), (2) are the same as in Example 1.

[0078] (3) Preparation of the test solution: Take about 5g of this product, accurately weigh it, accurately add 40ml of 3.0mol / L hydrochloric acid methanol solution (the volume ratio of hydrochloric acid to methanol is 2.7:10), weigh the weight, and heat to reflux for 60 Minutes, let cool, weighed again, made up for the lost weight with methanol solution, shaken up, filtered, accurately measured 4ml of the filtrate, put it in a volumetric bottle, diluted to 5ml with ethanol, shaken up, and used 0.45μm Filter through a microporous membrane to obtain.

[0079] (4) Determination method: each 10 μ l of the reference substance solution and the test solution are accurately drawn, injected into the liq...

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Abstract

The invention provides a method for measuring the content of luteolin in lamiophlomis rotata by liquid chromatography. The method comprises the following steps that the octadecylsilane chemically bonded silica is taken as a filling agent and the acetonitrile-tetrahydrofuran-0.5 percent of phosphoric acid is taken as the mobile phase; under the chromatographic conditions that the detected wavelength is 350 plus or minus 2 nm, the column temperature is 25 DEG C to 50 DEG C, the flow velocity is 0.5 ml / min to 1.5ml / min and the sample size is 5 mul to 20 mul, the liquid chromatography analysis is carried out on the prepared test solution, the chromatographic peak area of the corresponding position of the reference solution is measured, and the corresponding content is calculated according to the standard curve. The measuring method has the advantages of high precision, good reproducibility, high recovery ratio and accurate measuring result, improves the quality standard of the pharmaceutical preparation containing the lamiophlomis rotata herb, facilitates the quality stability and the quality control of the industrial production and ensures the security and the validity on medication use by people.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicines and relates to a method for detecting medicines, in particular to a method for measuring the content of luteolin in unique medicine preparations by high performance liquid chromatography. Background technique [0002] Luteolin (C 15 h 10 o 6 ) is a weakly acidic four-hydroxyflavone compound, which is a yellow crystal and belongs to flavonoids. Melting point of luteolin: 328°C~330°C (monohydrate), slightly soluble in water, soluble in alkali solution (monohydrate). [0003] Duyiwei is a traditional Tibetan medicine, and related preparations are widely used clinically for analgesia and hemostasis after various surgical operations, as well as for the treatment of stomatology, gynecology, and arthritis. "Chinese Pharmacopoeia" requires the determination of total flavonoids and luteolin content in Duyiwei and its preparations, and sets quality standards. A large number of pharmacologic...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 包旭宏张国霞李智勤桑杰东主
Owner GANSU CHEEZHENG TIBETAN MEDICINE CO LTD
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