Method for separating and determining tetrandrine and fangchinoline

A technology of fangchinoline and tetrandrine, which is applied in material separation, measuring devices, and analysis of materials, can solve the problems of unsuitable quality control methods for conventional drug preparations, long analysis time, and complicated equipment, and achieve low cost, The effect of high sensitivity and easy operation

Inactive Publication Date: 2015-01-21
复旦大学附属华东医院
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The above methods all use special reagents, expensive and complicated equipment, and the analysis time is also long, so v

Method used

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  • Method for separating and determining tetrandrine and fangchinoline
  • Method for separating and determining tetrandrine and fangchinoline
  • Method for separating and determining tetrandrine and fangchinoline

Examples

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Embodiment 1

[0030] Determination of Tetrandrine and Fangchinoline in Qifangxibifang Granules

[0031] 1. Sample pretreatment: Accurately weigh 0.8g of Qifangxibifang Granules, place it in a conical flask, add 25ml of methanol, stopper the bottle tightly, weigh, after ultrasonic for 30min, weigh, and make up the weight with methanol, Filter with a 0.45 μm filter membrane and inject 10 μL.

[0032] 2. Chromatographic conditions:

[0033] HPLC system:

[0034] Agilent 1200 HPLC system: including G1311A quaternary intake pump, G1329A automatic injector, G1322A online degasser and G1315B UV detector. Data were collected and analyzed with Agilent Workstation software (version B.02.01, Germany). Chromatographic column: ATENA C18 column (250 mm×6 mm inner diameter, 5 μM, Anpu Company, China), with a 0.5 μM pre-column filter. Add 1 g / L sodium octane sulfonate and filter with a 0.45 μm filter membrane before use. Mobile phase: methanol-water (65:35, V / V, adjust pH to 3 with glacial acetic acid...

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Abstract

The invention relates to a method for separating and determining tetrandrine and fangchinoline. The method comprises the following steps: 1, dissolving a Stephania tetrandra root raw drug or a traditional Chinese medicinal preparation containing the Stephania tetrandra root in methanol, carrying out ultrasonic treatment, and filtering; and 2, carrying out high performance liquid chromatography detection on the filtrate obtained in step 1, wherein the mobile phase is a methanol-water mixed solution with the volume ratio of 65:35, 1g/L of sodium octanesulfonate is added, the pH value is adusted by acetate acid gracial to 3, the flow velocity is 1mL/min, and the sample introduction amount is 10[mu]L. The method adopting methanol dissolving to carry out sample pretreatment has the advantages of simple operation and low cost, the whole chromatography process time is 14min, the lowest detection limits of tetrandrine and fangchinoline are 0.28mg/L and 0.13mg/L respectively, the linear ranges of the tetrandrine and fangchinoline are 125-4000mg/L and 47-1500mg/L respectively, the linear correlation coefficient is good, the recovery rate of the method is greater than 90%, and RSD is less than 10%.

Description

technical field [0001] The invention relates to the field of separation and determination of alkaloids, in particular to a method for separation and determination of tetrandrine and tetrandrine. Background technique [0002] Fangji, its main active monomers are tetrandrine and fangchinoline, which belong to alkaloids, have similar chemical structures, and are highly polar, so they cannot be effectively separated under ordinary HPLC conditions. In Fangji crude drugs and Chinese medicine preparations containing Fangji, the current analytical methods for the determination of tetrandrine and fangchinoline include capillary electrophoresis, flow injection micellar electrokinetic capillary chromatography system, ultraviolet high performance liquid chromatography, electrochemical detection and mass spectrometry . [0003] The above methods all use special reagents, expensive and complicated equipment, and the analysis time is also long, so various drawbacks make the above methods ...

Claims

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Application Information

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IPC IPC(8): G01N30/74G01N30/06
Inventor 卢新刚吴弢沈杰高翔杨涛傅峰苟海辛瞿佶李蠡王文昊朱斌
Owner 复旦大学附属华东医院
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