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Thirst quenching clearing particle content detection method

A detection method, the technology of Xiaokeqing, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of inability to fully characterize the integrity and complexity of traditional Chinese medicine preparations, and achieve the effect of accurate control

Active Publication Date: 2015-05-13
TIANJIN TASLY PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, under the content determination item of the quality standard of Xiaokeqing Granules, only the content of smilagenin in the hydrolyzate of Anemarrhena is determined, which cannot fully characterize the integrity and complexity of traditional Chinese medicine preparations. The active ingredients are complex and diverse. It is necessary to find a method that can detect multiple ingredients in order to effectively control the content and quality of the product in the production process. For this reason, the inventor has carried out experiments on various detection methods , and finally obtained a method suitable for Xiaokeqing Granules, and determined the content of the five components with high content, neomangiferin, mangiferin, timosaponin BII, palmatine and berberine

Method used

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  • Thirst quenching clearing particle content detection method
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  • Thirst quenching clearing particle content detection method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0092] Instruments and reagents

[0093] ACQUITY UPLC (Waters, USA, including quaternary high-pressure gradient pump, vacuum degasser, autosampler, column oven, PDA detector, Empower3 chromatography workstation), evaporative light scattering detector (ELSD) (Alltech ELSD2000), KQ-500DE CNC ultrasonic cleaner (Kunshan Ultrasonic Instrument Co., Ltd.), analytical balance (XS105 electronic analytical balance, Mettler Toledo), Millipore Simplicity ultrapure water system.

[0094] Acetonitrile, methanol (chromatographic grade, Merck); glacial acetic acid (chromatographic grade, Tianjin Concord Co., Ltd.); triethylamine (chromatographically pure, Tianjin Yuanli Chemical Co., Ltd.); absolute ethanol (analytical grade, Lian Longbohua Tianjin Pharmaceutical Chemical Co., Ltd.); reference substances of mangiferin (batch number 111607-200402), timosaponin BII (batch number 222839-201102) and berberine (batch number 110713-201212) were purchased from China National Institutes for Food and...

Embodiment 2

[0105] 1. A detection method for Xiaokeqing preparation, comprising the following steps:

[0106] Preparation of the test solution:

[0107] Take 1 g of Qukeqing preparation, and use 50% ethanol for ultrasonic extraction, and the ultrasonic time is 20 minutes.

[0108] Then add a solvent to adjust the solution concentration, filter through a microporous membrane, get the filtrate, and obtain it.

[0109] Preparation of reference substance stock solution:

[0110] Take appropriate amount of reference substances of neomangiferin, mangiferin, timosaponin BII, palmatine, and berberine, weigh them accurately, add 75% methanol to dissolve, and obtain mass concentrations of 0.244, 0.784, 0.772, 0.070, and 0.224 μg, respectively. µL -1 stock solution of the reference substance.

[0111] Content determination:

[0112] Inject the above-mentioned test solution and reference substance stock solution into the UPLC-PDA-ELSD chromatograph respectively to obtain a chromatogram. Accordin...

Embodiment 3

[0125] 1. A detection method for Xiaokeqing preparation, comprising the following steps:

[0126] Preparation of the test solution:

[0127] Take 7g of Qukeqing preparation, and use 80% ethanol for ultrasonic extraction, and the ultrasonic time is 40min.

[0128] Preparation of reference substance stock solution:

[0129] Take appropriate amount of reference substances of neomangiferin, mangiferin, timosaponin BII, palmatine, and berberine, weigh them accurately, add 75% methanol to dissolve, and obtain mass concentrations of 0.244, 0.784, 0.772, 0.070, and 0.224 μg, respectively. µL -1 stock solution of the reference substance.

[0130] Content determination:

[0131] Inject the above-mentioned test solution and reference substance stock solution into the UPLC-PDA-ELSD chromatograph respectively to obtain a chromatogram. According to the chromatogram, use the peak area method to calculate neomangiferin, mangiferin, and timosaponin BII in the test solution. , the content ...

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Abstract

The invention relates to a thirst quenching clearing particle content detection method, the method comprises the following steps: preparation of a to-be-tested sample solution, to be more specific, taking a thirst quenching clearing preparation, adding proper amount of extraction solvent methanol or ethanol, ultrasonically dissolving, adding a solvent to adjust the solution concentration, filtering with a microfiltration membrane to obtain filtrate; preparation of a control stock solution, to be more specific, taking neomangiferin, mangiferin, timosaponin BII, palmatine and berberine controls, adding methanol for dissolving to obtain the control stock solution; determination of content, to be more specific, respectively injecting the to-be-tested sample solution and the control stock solution into UPLC-PDA-ELSD chromatograph to obtain a chromatogram, and according to the chromatogram, using the peak area method for calculation of content of the neomangiferin, mangiferin, timosaponin BII, palmatine and berberine.

Description

Technical field: [0001] The present invention relates to a method for determining the active ingredient of medicine, in particular to a method for detecting the content of active ingredient of medicine in Xiaokeqing granule Background technique: [0002] Xiaokeqing granule is a Chinese patent medicine for treating diabetes already on the market. Its formula is composed as follows: Anemarrhena anemarrhena, Atractylodes atractylodes, Coptis chinensis, Puhuang, Dijincao, and appropriate amount of auxiliary materials. The preparation method includes the following steps: [0003] (a) Take Anemarrhena, Cangzhu, Coptis Rhizoma, Puhuang, Dijincao, and spare; [0004] (b) Atractylodes atractylodis extracts volatile oil by steam distillation for 5 hours, then clathrates atractylodes volatile oil with β-cyclodextrin, feeds atractylodes atractylodis oil and β-cyclodextrin at a ratio of 1:6, and dries at 50°C to obtain β-cyclodextrin The fine clathrate is set aside, and the extract is f...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 佟玲周水平孙鹤李东翔王露黔李晓稳
Owner TIANJIN TASLY PHARMA CO LTD
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