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Analysis method for four anthraquinones in blood plasma and application of four anthraquinones in pharmacokinetics

A blood plasma and method quantitative technology, applied in the direction of analysis of materials, scientific instruments, material separation, etc., can solve the problem of simultaneous detection and achieve high sensitivity and accurate detection results

Active Publication Date: 2014-02-12
北京中一堂科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Emodin, aloe-emodin, chrysophanol and emodin methyl ether are the four active ingredients in Tangminlin, but there is no method that can simultaneously detect these four ingredients in plasma samples

Method used

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  • Analysis method for four anthraquinones in blood plasma and application of four anthraquinones in pharmacokinetics
  • Analysis method for four anthraquinones in blood plasma and application of four anthraquinones in pharmacokinetics
  • Analysis method for four anthraquinones in blood plasma and application of four anthraquinones in pharmacokinetics

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0116] LC-MS / MS conditions

[0117] Column: Hypersil Gold-C 18 (150×2.1mm, 5μm, Thermo)

[0118] Pre-column: Security Guard-C 18 (4.0mm×3.0mm i.d,5μm,Phenomenex)

[0119] Mobile phase: acetonitrile-0.05% ammonia solution (70:30)

[0120] Column temperature: 25℃

[0121]Flow rate: 250μL·min -1

[0122] Ion source: Electrospray ionization source (ESI)

[0123] Ionization mode: negative ion mode

[0124] MS / MS: Selective Reaction Monitoring (SRM). The ion reactions used for quantitative analysis were m / z239→211 (internal standard, 1,8-dihydroxyanthraquinone), m / z253→225 (chrysophanol), m / z269→225 (emodin), m / z z269→240 (Aloe-emodin), m / z283→240 (Emodin methyl ether).

[0125] Mass spectrometry parameters: spray voltage: 3500V; ion source voltage: 10eV; capillary temperature: 350°C; sheath gas: N 2 (35psi); auxiliary gas: N 2 (10psi); collision gas pressure: Ar1.0mTorr (1Torr=133.3Pa); collision-induced fragmentation (CID) voltages of 1,8-dihydroxyanthraquinone, chryso...

Embodiment 2

[0134] LC-MS / MS conditions

[0135] Column: Hypersil Gold-C 18 (150×2.1mm, 5μm, Thermo)

[0136] Pre-column: Security Guard-C 18 (4.0mm×3.0mm i.d,5μm,Phenomenex)

[0137] Mobile phase: acetonitrile-0.05% ammonia solution (70:30)

[0138] Column temperature: 25℃

[0139] Flow rate: 250μL·min -1

[0140] Ion source: Electrospray ionization source (ESI)

[0141] Ionization mode: negative ion mode

[0142] MS / MS: Selective Reaction Monitoring (SRM). The ion reactions used for quantitative analysis were m / z239→211 (internal standard, 1,8-dihydroxyanthraquinone), m / z253→225 (chrysophanol), m / z269→225 (emodin), m / z z269→240 (Aloe-emodin), m / z283→240 (Emodin methyl ether).

[0143] Mass spectrometry parameters: spray voltage: 3000V; ion source voltage: 10eV; capillary temperature: 350°C; sheath gas: N 2 (35psi); auxiliary gas: N 2 (20psi); collision gas pressure: Ar1.0mTorr (1Torr=133.3Pa); collision-induced fragmentation (CID) voltages of 1,8-dihydroxyanthraquinone, chrys...

Embodiment 3

[0150] LC-MS / MS conditions

[0151] Column: Hypersil Gold-C 18 (100×2.1mm, 5μm, Thermo)

[0152] Pre-column: Security Guard-C 18 (4.0mm×3.0mm i.d,5μm,Phenomenex)

[0153] Mobile phase: acetonitrile-0.05% ammonia solution (70:30)

[0154] Column temperature: 25℃

[0155] Flow rate: 300μL·min -1

[0156] Ion source: Electrospray ionization source (ESI)

[0157] Ionization mode: negative ion mode

[0158] MS / MS: Selective Reaction Monitoring (SRM). The ion reactions used for quantitative analysis were m / z239→211 (internal standard, 1,8-dihydroxyanthraquinone), m / z253→225 (chrysophanol), m / z269→225 (emodin), m / z z269→240 (Aloe-emodin), m / z283→240 (Emodin methyl ether).

[0159] Mass spectrometry parameters: spray voltage: 2500V; ion source voltage: 10eV; capillary temperature: 350°C; sheath gas: N 2 (45psi); auxiliary gas: N 2 (15psi); collision gas pressure: Ar1.0mTorr (1Torr=133.3Pa); collision-induced fragmentation (CID) voltages of 1,8-dihydroxyanthraquinone, chrys...

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Abstract

The invention discloses an analysis method for determining rheum emodin, aloe-emodin, chrysophanol and emodin monomethyl ether in blood plasma at the same time and application of rheum emodin, aloe-emodin, chrysophanol and emodin monomethyl ether in pharmacokinetics, wherein the analysis method for determining rheum emodin, aloe-emodin, chrysophanol and emodin monomethyl ether in the blood plasma at the same time comprises the following steps: (1) preparing a sample; (2) detecting. The analysis method for determining rheum emodin, aloe-emodin, chrysophanol and emodin monomethyl ether in the blood plasma at the same time has good specificity, high precision degree, high accuracy and wide linear range and can be used for in vivo pharmacokinetic determination of Chinese medicinal compositions.

Description

technical field [0001] The invention belongs to the application field of modern traditional Chinese medicine, and particularly relates to an LC-MS / MS detection method for emodin, aloe-emodin, chrysophanol and emodin methyl ether in plasma, and an application in pharmacokinetics. Background technique [0002] Mass spectrometry is an analytical method based on molecular weight determination. In recent years, its combination with separation mechanisms such as high performance liquid chromatography (HPLC) or capillary electrophoresis (CE) not only improves its ability to resist impurities and saves analysis time, and greatly improved the sensitivity of the assay. The development of soft ionization techniques, such as electrospray ionization (ESI), has expanded the scope of molecular weight detection. In addition, electrospray ionization technology can be carried out at atmospheric pressure, which is convenient to connect with liquid chromatography, making liquid chromatography-...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/02G01N30/34
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
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