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A detection method for lignans and flavonol glycosides in ginkgo biloba extract or its preparation

A flavonol glycosides and detection method technology, which is applied in the detection field of ginkgo biloba extract, can solve the problems that cannot be quantitatively detected at the same time, achieve the effects of improving and controlling quality, simplifying the inspection process, and high precision and accuracy

Active Publication Date: 2021-09-28
SHINEWAY PHARMA GRP LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing high-performance liquid chromatography detection method cannot simultaneously quantitatively detect lignans (aricine-4,4-diglucoside and pinoresinol diglucoside) and flavonol glycosides in Ginkgo biloba extract or its preparations For the content of lignans (Urolignoside and cosmoside), the invention provides a detection method for lignans and flavonol glycosides in Ginkgo biloba extract or its preparation

Method used

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  • A detection method for lignans and flavonol glycosides in ginkgo biloba extract or its preparation
  • A detection method for lignans and flavonol glycosides in ginkgo biloba extract or its preparation
  • A detection method for lignans and flavonol glycosides in ginkgo biloba extract or its preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Materials and Methods

[0031] Instrument: Waters Xevo GX-XS quadrupole tandem time-of-flight mass spectrometer

[0032] Reagents: acetonitrile, methanol (chromatographically pure), purified water, and other reagents are of analytical grade; agaricin-4,4-diglucoside, pinoresinol diglucoside, Urolignoside and cosmoside reference substances

[0033] Samples: Ginkgo biloba extract, Shuxuening injection

[0034] Solution preparation:

[0035] Preparation of reference solution:

[0036] Precisely weigh 12.16mg of agaricin-4,4-diglucoside in a 50ml volumetric flask, 10.90mg of pinoresinol diglucoside in a 50ml volumetric flask, 9.20mg of Urolignoside in a 50ml volumetric flask, and 10.26mg of cosmoside in a 50ml volumetric flask bottle, dissolved in methanol and made to volume, as the mother solution of the reference substance. Precisely measure 2ml of agaricin-4,4-diglucoside, 2ml of pinoresinol diglucoside, 5ml of Urolignoside and 1ml of cosmoside reference substance mo...

Embodiment 2

[0046] Methodological investigation and results

[0047] Linear relationship: Dilute the mixed reference solution 2 times, 5 times, 10 times, 20 times and 40 times respectively, precisely draw 1 μL of the mixed reference solution and the above-mentioned diluted solution into the liquid chromatograph, and extract each component to be tested The exact molecular weight was recorded and the peak area was recorded.

[0048] Wherein, the results of linear relationship investigation of agaricin-4,4-diglucoside are shown in Table 1;

[0049] Table 1 Investigation of the linear relationship of agaricin-4,4-diglucoside

[0050]

[0051]

[0052] According to the above table, with the injection volume (ug) as the abscissa (X), and the peak area as the ordinate (Y), draw a standard curve to obtain the regression equation of agaricin-4,4-diglucoside as:

[0053] y=23574.7465x+35594.1644, R2=0.9997 (n=6). It shows that agaricin-4,4-diglucoside in the reference substance has a good li...

Embodiment 3

[0102] The UPLC-MS method in Example 1 was used to detect the contents of agaricin-4,4-diglucoside, pinoresinol diglucoside, Urolignoside and cosmoside in the Ginkgo biloba extract.

[0103] Get 10 batches of Ginkgo biloba extracts, 2 parts per batch, prepare the solution to be tested according to the preparation method of the Ginkgo biloba extract test solution in Example 1, accurately draw 1ul into the chromatograph, and extract the precise molecular weight of each component to be tested , record the peak area, and calculate the content of each component to be tested in the Ginkgo biloba extract, and the content detection results are shown in Table 15-18.

[0104] Table 15 Determination results of agaricin-4,4-diglucoside content in Ginkgo biloba extract

[0105]

[0106]

[0107] Determination results of pinoresinol diglucoside content in table 16 Ginkgo biloba extract

[0108]

[0109]

[0110] Table 17 Determination results of Urolignoside content in Ginkgo b...

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Abstract

The invention relates to the technical field of detection of Ginkgo biloba extract, and specifically discloses a detection method for lignans and flavonol glycosides in Ginkgo biloba extract or its preparations. The detection method is UPLC-MS method, wherein UPLC The detection conditions are: chromatographic column: octadecylsilane bonded silica gel column; mobile phase: mobile phase A is acetonitrile, mobile phase B is 0.08‑0.12vt% formic acid aqueous solution, and the volume ratio of mobile phase A to mobile phase B is 10-35:90-60; column temperature: 35-40°C; flow rate: 0.1-0.5ml / min; elution method: isocratic elution; the detection mode of the MS is negative ion mode. The present invention can realize the simultaneous quantitative detection of two lignan compounds and two flavonol glycoside compounds in ginkgo biloba extract with complex components or its preparation, and the detection precision and accuracy are high and reproducible and good stability.

Description

technical field [0001] The invention relates to the technical field of detection of ginkgo leaf extracts, in particular to a detection method for lignans and flavonol glycosides in ginkgo leaf extracts or preparations thereof. Background technique [0002] Ginkgo biloba extract is an effective substance extracted from Ginkgo biloba. It contains ginkgo total flavonoids, ginkgolides and other substances, which can expand blood vessels, protect vascular endothelial tissue, regulate blood lipids, protect low-density lipoproteins, and inhibit PAF (platelet activating factor) , Inhibit thrombosis, scavenge free radicals and so on. Among them, the ingredients that play the role of scavenging free radicals are lignans; the main ingredients that play the role of expanding blood vessels, protecting vascular endothelial tissue, and regulating blood lipids are flavonol glycosides. Therefore, lignans in Ginkgo biloba extract or its preparations The content of ketone compounds and flavon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/54
CPCG01N30/02G01N30/06G01N30/54G01N30/72G01N2030/027G01N2030/062
Inventor 李玉彩李响明杨琴周永妍王文鹏王雪莲孙胜斌姜国志
Owner SHINEWAY PHARMA GRP LTD
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