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A method for simultaneous determination of flavonoids and lactones in ginkgo extract and its preparation

A technology for Ginkgo biloba extract and preparation, which is applied in the field of high performance liquid chromatography-mass spectrometry and can solve the problems of low sensitivity, solvent consumption, and inability to fully represent the properties of injections.

Active Publication Date: 2021-09-10
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

[0003] In the current detection method, the flavonoids and lactones 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; (quercetin, kaempferol, isorhamnetin), which cannot fully represent the properties of the 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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  • A method for simultaneous determination of flavonoids and lactones in ginkgo extract and its preparation
  • A method for simultaneous determination of flavonoids and lactones in ginkgo extract and its preparation
  • A method for simultaneous determination of flavonoids and lactones in ginkgo extract and its preparation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Sample treatment: Shuxuening injection was diluted 20 times with 50% methanol / 50% water.

[0036] (2) Ultra-high performance liquid chromatography-mass spectrometry method

[0037] 1) Ultra-high performance liquid chromatography analysis method

[0038] The ultra-high performance liquid chromatograph is Waters UPLC Acquity UPLC I-CLASS, including a quaternary solvent manager, an automatic sampler, a column thermostat and an Empower chromatography workstation; 16 kinds of flavonoids and 4 kinds of lactone reference substances are self-made and Confirmed by structure and purity. Formic acid was a product of Sigma, USA; acetonitrile was chromatographically pure; water was Millpore ultrapure water.

[0039] Chromatographic conditions:

[0040] Chromatographic column: Acquity UPLC BEH Shield RP18 column (2.1×100mm)

[0041] Mobile phase: A, acetonitrile; B, water-0.1% formic acid

[0042] Gradient: 12%A to 38%A in 10min

[0043] Flow rate: 0.3mL / min

[0044] Colum...

Embodiment 2

[0068] Change the sample of the (three) section in embodiment 1 into B sample, and others are the same as embodiment 1.

[0069] (3) Determination of actual Shuxuening injection sample content

[0070] The Shuxuening injection sample from manufacturer B was analyzed according to the above-mentioned ultra-high performance liquid chromatography-mass spectrometry method. The determination results of 20 compounds are shown in Table 5, and the RSD is less than 5% (n=3).

Embodiment 3

[0072] Change the sample of the (three) section in embodiment 1 into C sample, and others are the same as embodiment 1.

[0073] (3) Determination of actual Shuxuening injection sample content

[0074] The Shuxuening injection sample from manufacturer C was analyzed according to the above-mentioned ultra-high performance liquid chromatography-mass spectrometry method. The determination results of 20 compounds are shown in Table 5, and the RSD is less than 5% (n=3).

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Abstract

The invention relates to a high-performance liquid chromatography-mass spectrometry method for simultaneous and rapid determination of flavonoids and lactones in ginkgo extract and its preparation. The method comprises the following steps: diluting the sample with 50% methanol / 50% water; utilizing RP-HPLC method to carry out the determination of flavonoids and lactones, and establishing the HPLC-MS simultaneous determination method of 16 kinds of flavonoids and 4 kinds of lactones in the ginkgo extract preparation , the mobile phase selected in the determination process was composed of acetonitrile and water, the flow rate was 0.3mL / min, the column temperature was 35°C, the injection volume was 5μL, and the mass spectrometry selected ion monitoring (MRM) mode was used for detection; 16 kinds of flavonoids and 4 kinds of lactones were used as The standard sample was used to establish the linear equation of the HPLC-MS determination method. The method is fast, simple, accurate and reliable, and stable, and is suitable for the simultaneous qualitative and quantitative analysis of flavonoids and lactones in Ginkgo biloba extract and its preparations.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography-mass spectrometry method for simultaneous and rapid determination of flavonoids and lactones in ginkgo extracts and preparations thereof. It is characterized in that: the sample is diluted with 50% methanol / 50% water; the determination of flavonoids and lactones is carried out by using RP-HPLC method, and the simultaneous determination method of 16 kinds of flavonoids and 4 kinds of lactones in ginkgo extract preparation is established by HPLC-MS , the mobile phase selected during the determination is composed of acetonitrile and water, the chromatographic column is an Acquity UPLC BEH Shield RP18 column, the flow rate is 0.3mL / min, the column temperature is 35°C, the injection volume is 5μL, and the mass spectrometry selected ion monitoring (MRM) mode is detected; Using 16 flavonoids and 4 lactones as standard samples, a linear equation for the HPLC-MS determination method was established...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 梁鑫淼金高娃郭志谋
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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