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Analysis method of five flavonoid glycosides in plasma and its application in pharmacokinetics

A technology of plasma and baicalin, applied in liquid chromatography tandem mass spectrometry detection, in the application field of pharmacokinetics, to achieve high sensitivity and accurate detection results

Active Publication Date: 2016-08-10
北京中一堂科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Naringin, hesperidin, neohesperidin, baicalin and wogonoside are the five active ingredients in Tangminlin, but there is no method that can simultaneously detect these five ingredients in plasma samples

Method used

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  • Analysis method of five flavonoid glycosides in plasma and its application in pharmacokinetics
  • Analysis method of five flavonoid glycosides in plasma and its application in pharmacokinetics
  • Analysis method of five flavonoid glycosides in plasma and its application in pharmacokinetics

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0123] LC-MS / MS conditions

[0124] Column: ZORBAX SB-C 18 (150×2.1mm, 5μm, Agilent)

[0125] Pre-column: Security Guard-C 18 (4.0mm×3.0mm i.d, 5μm, Phenomenex)

[0126] Mobile phase: 0.1% formic acid water (A)-acetonitrile (B), gradient elution program: 0~3.0min, 24%B; 3.0~3.1min, 24%B–40%B; 3.1~10.0min, 40%B B-60% B.

[0127] Column temperature: 25°C

[0128] Flow rate: 300μL·min -1

[0129] Ion source: electrospray ionization source (ESI)

[0130] Ionization mode: positive and negative ion switching mode

[0131] MS / MS: Selected Reaction Monitoring (SRM). 0~4.0min, using negative ion mode, the ions used for quantitative analysis are m / z579→271 (naringin), m / z609→301 (hesperidin and neohesperidin), m / z417→255 ( Internal standard, liquiritin); 4.1~10.0min, using positive ion mode, the ions used for quantitative analysis were m / z447→271 (baicalin), m / z461→285 (wogonin).

[0132] Mass spectrometry parameters: In negative ion mode, the parameter spray voltage is 4000V...

Embodiment 2

[0141] LC-MS / MS conditions

[0142] Column: ZORBAX SB-C 18 (150×2.1mm, 5μm, Agilent)

[0143] Pre-column: Security Guard-C 18 (4.0mm×3.0mm i.d, 5μm, Agilent)

[0144] Mobile phase: 0.01% formic acid water (A)-acetonitrile (B), gradient elution program: 0~3.0min, 30%B; 3.0~3.1min, 24%B–60%B; 3.1~10.0min, 60%B B – 80% B.

[0145] Column temperature: 20°C

[0146] Flow rate: 250μL·min -1

[0147] Ion source: electrospray ionization source (ESI)

[0148] Ionization mode: positive and negative ion switching mode

[0149] MS / MS: Selected Reaction Monitoring (SRM). 0~4.0min, using negative ion mode, the ions used for quantitative analysis are m / z579→271 (naringin), m / z609→301 (hesperidin and neohesperidin), m / z417→255 ( Internal standard, liquiritin); 4.1~10.0min, using positive ion mode, the ions used for quantitative analysis were m / z447→271 (baicalin), m / z461→285 (wogonin).

[0150] Mass spectrometry parameters: In negative ion mode, the parameter spray voltage is 4000V...

Embodiment 3

[0157] LC-MS / MS conditions

[0158] Chromatographic column: WondaSil-C18 (150×2.1mm, 5μm, Shimadzu)

[0159] Pre-column: Security Guard-C 18 (4.0mm×3.0mm i.d, 5μm, Phenomenex)

[0160] Mobile phase: 0.5% formic acid water (A)-acetonitrile (B), gradient elution program: 0~3.0min, 24%B; 3.0~3.1min, 24%B–60%B; 3.1~10.0min, 60%B b.

[0161] Column temperature: 30°C

[0162] Flow rate: 300μL·min -1

[0163] Ion source: electrospray ionization source (ESI)

[0164] Ionization mode: positive and negative ion switching mode

[0165] MS / MS: Selected Reaction Monitoring (SRM). 0~4.0min, using negative ion mode, the ions used for quantitative analysis are m / z579→271 (naringin), m / z609→301 (hesperidin and neohesperidin), m / z417→255 ( Internal standard, liquiritin); 4.1~10.0min, using positive ion mode, the ions used for quantitative analysis were m / z447→271 (baicalin), m / z461→285 (wogonin).

[0166] Mass spectrometry parameters: In negative ion mode, the parameter spray voltage ...

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Abstract

The present invention provides a method for the quantitative detection of naringin, hesperidin, neohesperidin, baicalin and wogonin in plasma samples by liquid chromatography tandem mass spectrometry, including the preparation of the sample in step (1) and the step ( 2) Detection. The analysis method of the invention has good specificity, high precision and accuracy, and wide linear range, and can be used for pharmacokinetic determination of traditional Chinese medicine compositions in vivo.

Description

technical field [0001] The invention belongs to the application field of modern traditional Chinese medicines, and in particular relates to a liquid chromatography tandem mass spectrometry detection method for five flavonoid glycosides in blood plasma and an application in pharmacokinetics. Background technique [0002] Mass spectrometry is an analysis method based on the determination of molecular weight. In recent years, its combination with separation mechanisms such as high performance liquid chromatography (HPLC) or capillary electrophoresis (CE) has not only improved its ability to resist interference from impurities and saved analysis time. time, and greatly improved the sensitivity of the assay. The development of soft ionization techniques, such as electrospray ionization (ESI), has expanded the range of molecular weight detection. In addition, electrospray ionization technology can be carried out under atmospheric pressure, which is convenient to connect with liqu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/72
Inventor 佟玲周水平朱永宏马晓慧靳元鹏鄂秀辉
Owner 北京中一堂科技有限公司