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Method for simultaneously determining components in ginkgo biloba extract and preparation thereof

A technique for Ginkgo biloba extract and preparation, which is applied in the field of analytical chemistry, can solve the problems that the properties of injections cannot be fully represented, the possible content of a single peak varies greatly, and the solvent consumption is large, etc., and achieves low reagent dosage, strong sensitivity and low cost. Effect

Pending Publication Date: 2021-02-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the current detection method, flavonoids, lactones and ginkgolic acid are measured separately, which takes a long time and consumes a lot of solvent; when using ELSD detection, the sensitivity is low and the repeatability is poor; Flavonoid aglycones (quercetin, kaempferol, isorhamnetin) cannot fully represent the properties of injections. Even if the total amount of flavonoids in different injections is similar, the content of each single peak may vary greatly

Method used

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  • Method for simultaneously determining components in ginkgo biloba extract and preparation thereof
  • Method for simultaneously determining components in ginkgo biloba extract and preparation thereof
  • Method for simultaneously determining components in ginkgo biloba extract and preparation thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1). Sample treatment: Shuxuening injection was diluted 50 times with 50% methanol / 50% water.

[0035] (2). Ultra-high performance liquid chromatography-mass spectrometry method

[0036] 1) Ultra-high performance liquid chromatography analysis method

[0037] The ultra-high performance liquid chromatograph is Shimadzu Nexera X2, including a binary solvent manager, an automatic sampler, and a column thermostat; 17 kinds of flavonoids, 5 kinds of lactones and 5 kinds of ginkgolic acid reference substances are self-made or purchased in the laboratory, And through the structure, purity confirmation. Formic acid was a product of Sigma, USA; acetonitrile was chromatographically pure; water was Millpore ultrapure water.

[0038] Chromatographic conditions:

[0039] Instrument: UHPLC for Shimadzu Nexera X2 system

[0040] Chromatographic column: Acquity UPLC HSS T3 column (2.1×100mm)

[0041] Mobile phase: A, acetonitrile-0.5% formic acid; B, water-0.5% formic acid

[004...

Embodiment 2

[0073] Change the sample of the (three) section in embodiment 1 into B sample, and others are the same as embodiment 1.

[0074] (3) Determination of actual Shuxuening injection sample content

[0075] The Shuxuening injection samples from manufacturer B were analyzed according to the above ultra-high performance liquid chromatography-mass spectrometry method, and the determination results of 27 compounds are shown in Table 5.

Embodiment 3

[0077] Change the sample of the (three) section in embodiment 1 into C sample, and others are the same as embodiment 1.

[0078] (3) Determination of actual Shuxuening injection sample content

[0079] The Shuxuening injection samples from manufacturer C were analyzed according to the above ultra-high performance liquid chromatography-mass spectrometry method, and the determination results of 27 compounds are shown in Table 5.

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Abstract

The invention relates to a method for simultaneously and rapidly determining components in a ginkgo biloba extract and a preparation thereof. The method comprises the following steps: diluting a sample with 50% methanol / 50% water; determining flavones, lactones and ginkgolic acid by using an RP-HPLC method, establishing an HPLC-MS simultaneous determination method for 17 flavones, 5 lactones and 5ginkgolic acids in the ginkgo biloba extract preparation, wherein a mobile phase selected in the determination process is composed of acetonitrile and water, a chromatographic column is an Acquity UPLC HSS T3 column, the flow velocity is 0.45 mL / min, the column temperature is 40 DEG C, the sample size is 5 [mu] L, and a mass spectrum selects an ion monitoring (MRM) mode for detection; 17 flavonoids, 5 lactones and 5 ginkgolic acids are taken as standard samples, and a linear equation of the HPLC-MS determination method is established. The method has the characteristics of rapidness, simplicity, accurate and reliable result, good stability and the like, and is suitable for simultaneous qualitative and quantitative analysis of flavones, lactones and ginkgolic acid compounds in the ginkgo biloba extract and preparation thereof.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a high-performance liquid chromatography-mass spectrometry method for simultaneous and rapid determination of flavonoids, lactones and ginkgolic acid in ginkgo extracts and preparations thereof. [0002] technical background [0003] Ginkgo biloba extract is used for ischemic cardiovascular and cerebrovascular diseases, coronary heart disease, angina pectoris, cerebral embolism, cerebral vasospasm, etc. Its clinical medicines include injections, tablets, granules, etc. The active ingredients are mainly flavonoids and lactones, and ginkgolic acid is the harmful ingredient. Liquid chromatography is mainly used in its quality control, wherein flavonoids and ginkgolic acids are detected by ultraviolet light, and lactone compounds are detected by evaporative light scattering detector (ELSD) because they have no ultraviolet absorption. For flavonoids, due to the lack of ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/04G01N30/06
CPCG01N30/02G01N30/72G01N30/04G01N30/06G01N2030/042
Inventor 梁鑫淼金高娃宋春颖郭志谋
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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