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Method for measuring mangiferin and bergenin in heat-clearing cough-relieving syrup in manner of liquid mass spectrum serial connection

A technology of salicylic acid and mangiferin, which is applied in the field of liquid mass spectrometry tandem determination of mangiferin and salicylic acid in Qingre antitussive syrup, can solve the problems of affecting integration and misjudgment of sample quality, and achieves high specificity and good separation. , good reproducibility

Inactive Publication Date: 2016-08-17
WUZHOU INST FOR FOOD & DRUG CONTROL
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Problems solved by technology

Take another 450g of sucrose, add an appropriate amount of water and boil to dissolve, add the above concentrated solution, 2.5g of benzoic acid, 0.5g of ethylparaben (dissolve the benzoic acid and ethylparaben with a small amount of ethanol) and an appropriate amount of essence, add water to 1000ml, stir well, that is In actual work, according to the pharmacopoeia method, it is found on the sample chromatogram that under the isocratic chromatographic environment specified in the pharmacopoeia, the same situation as the baseline drift of the gradient condition chromatographic environment will appear, which will affect the integration of the component of the sample. The quality of the sample is misjudged, but the same chromatographic conditions do not have this situation in the chromatogram of the reference substance

Method used

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  • Method for measuring mangiferin and bergenin in heat-clearing cough-relieving syrup in manner of liquid mass spectrum serial connection

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Embodiment 1

[0023] A liquid-mass spectrometry tandem method for determining mangiferin and petrinin in heat-clearing and cough-relieving syrup, the detection method includes the following steps in sequence:

[0024] Precisely measure 1ml of this product, put it in a 10mL extraction pool, use methanol to extract the sample statically at 60°C for 3 minutes, repeat the extraction twice, after the extraction is completed, dilute the extract to 20mL with methanol, and pipette 1mL into a centrifuge tube vortex for 2 minutes, centrifuge at 15,000 r / min for 3 minutes, and take the supernatant for chromatographic analysis;

[0025] Described chromatographic conditions are as follows:

[0026] The chromatographic conditions are as follows:

[0027] Chromatographic column: Kromasil-C18 column, 50mm×4.6mm×5mm;

[0028] Mobile phase: methanol-acetonitrile-1mmol / L ammonium acetate solution, using gradient elution;

[0029] The gradient elution procedure is as follows: 0-1min, 85%-45%A, 10%B, 5%-45%C...

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Abstract

The invention provides a method for measuring mangiferin and bergenin in heat-clearing cough-relieving syrup in a manner of liquid mass spectrum serial connection. The invention aims to provide the method for measuring mangiferin and bergenin in heat-clearing cough-relieving syrup in the manner of liquid mass spectrum serial connection, which has the advantages of simple detection and high detection result accuracy. The method comprises the following steps: precisely taking 1ml sample; putting into a 10mL extraction pool; statically extracting the sample for 3min at 60 DEG C with methyl alcohol; repeatedly extracting for 2 times; after completing extraction, using methyl alcohol for keeping the constant volume of the extracting solution at 20mL; sucking the extracting solution into a 1mL centrifugal tube; swirling for 2min; centrifuging for 3min at the speed of 15000r / min; and taking the supernate and performing chromatographic analysis. The method belongs to the technical field of chemical detection.

Description

technical field [0001] The invention provides a liquid-mass spectrometry tandem method for measuring mangiferin and petracenin in heat-clearing and cough-relieving syrup; it belongs to the technical field of chemical detection. Background technique [0002] The heat-clearing and cough-relieving syrup is composed of 8 herbs, Tinglizi, Dwarf Tea, Houttuynia cordata, Nepeta, Peucedanum, chestnut shell, and pumice. It has the effect of clearing away heat and relieving phlegm. It is clinically used to treat cold, pharyngitis, For lung heat cough and other diseases, it is reported that Qingre Cough Syrup has different degrees of inhibitory effects on common bacteria in respiratory tract infections such as Staphylococcus aureus, beta-hemolytic streptococcus, and pneumococcus; Decoct twice, the first time for 2 hours, the second time for 1.5 hours, filter, combine the filtrate and concentrate to about 650ml, let it stand, filter, and the filtrate for later use. Take another 450g of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 陈学松陈江涛廖强梁慧敏李亚李澄
Owner WUZHOU INST FOR FOOD & DRUG CONTROL
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