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Method for determining salvianolic acid L in blood plasma

A technology of salvianolic acid and blood plasma, applied in the field of drug content in plasma, can solve the problems of low sensitivity, low content, complex structure of salvianolic acid L, etc.

Inactive Publication Date: 2014-09-24
TIANJIN TASLY PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] As a new drug, salvianolic acid L needs a lot of drug research work, including pharmacokinetic research, but because salvianolic acid L has a complex structure, poor stability, contains a large number of phenolic and acid groups, and its content is extremely low, It is difficult to accurately determine its presence and content in body fluids or solutions with existing technologies
[0010] Previously, some researchers established an HPLC quantitative method for salvianolic acid L, but this method has low sensitivity (50ng / mL), and has certain limitations in the determination of blood drug concentration under oral administration.

Method used

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  • Method for determining salvianolic acid L in blood plasma
  • Method for determining salvianolic acid L in blood plasma
  • Method for determining salvianolic acid L in blood plasma

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] Plasma sample pretreatment:

[0100] 200uL plasma + 50uL 1M hydrochloric acid + 20uL internal standard (rosmarinic acid), vortexed for 30s, added 3mL ethyl acetate, vortexed for 4min, centrifuged to take the ethyl acetate layer, and dried in a 30°C water bath with nitrogen. After drying, reconstitute with 100uL mobile phase (0.1% formic acid water: acetonitrile = 7:3), vortex for 3min, centrifuge at 12000r / min for 3min, take the supernatant and inject 20uL.

[0101] Determination conditions:

[0102] Chromatographic column: Agilent ZORBAX Eclipse XDB-C18Analytical 2.1×150mm3.5-Micron Mobile phase: A: 0.1% formic acid water, B: acetonitrile.

[0103] Elution conditions: 0-3.7min, A:B=70:30 (v / v) isocratic elution, flow rate 0.25mL / min.

[0104] Mass spectrometry conditions: negative ion scanning, spray voltage -3000V, shell gas 5arb, auxiliary gas 20arb, capillary temperature 350°C. SRM detection mode is used to detect ion pairs: salvianolic acid L m / z537-295, collisi...

Embodiment 2

[0106] Plasma sample pretreatment:

[0107] 200uL plasma + 50uL 0.01M hydrochloric acid + 20uL internal standard (rosmarinic acid), vortexed for 10s, added 1mL ethyl acetate, vortexed for 1min, centrifuged to take the ethyl acetate layer, and dried in a water bath with nitrogen at 10°C. After drying, reconstitute with 100uL mobile phase, vortex for 3min, centrifuge at 12000r / min for 1min, take supernatant and inject 20uL.

[0108] Determination conditions:

[0109] Chromatographic column: Agilent ZORBAX Eclipse XDB-C18Analytical 2.1×150mm3.5-Micron Mobile phase: A: 0.02% formic acid water, B: acetonitrile.

[0110] Elution conditions: 0-3.7min, A:B=30:70 (v / v) isocratic elution, flow rate 0.1mL / min.

[0111] Mass spectrometry conditions: negative ion scanning, spray voltage -2500V, shell gas 1arb, auxiliary gas 5arb, capillary temperature 250°C. SRM detection mode is used to detect ion pairs: salvianolic acid L m / z537-493, collision energy (CE)=5eV, rosmarinic acid m / z359-1...

Embodiment 3

[0113] Plasma sample pretreatment:

[0114] 200uL plasma + 50uL 5M sulfuric acid + 20uL internal standard (danshensu), vortexed for 3min, added 3mL of petroleum ether, vortexed for 10min, centrifuged to take the petroleum ether layer, and dried with nitrogen in a water bath at 60°C. After drying, reconstitute with 100uL mobile phase, vortex for 3min, centrifuge at 15000r / min for 10min, take supernatant and inject 20uL.

[0115] Determination conditions:

[0116] Chromatographic column: Agilent ZORBAX Eclipse XDB-C8Analytical2.1×150mm3.5-Micron Mobile phase: A: 5% formic acid water, B: acetonitrile.

[0117] Elution conditions: 0-3.7min, A:B=90:10 (v / v) isocratic elution, flow rate 0.4mL / min.

[0118] Mass spectrometry conditions: negative ion scanning, spray voltage -3500V, shell gas 15arb, auxiliary gas 30arb, capillary temperature 400°C. SRM detection mode was used to detect ion pairs: salvianolic acid L m / z537-185, collision energy (CE)=40eV, danshensu m / z197-135, CE=30e...

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Abstract

The invention relates to a method for determining content of medicine in blood plasma, which comprises the following steps: 1)treating a sample; taking the sample of blood plasma, adding a proper amount of an acid solution and an internal standard solution, mixing; adding an organic solvent for mixing and then extracting; centrifuging the above mixed liquor and taking an organic solvent layer, blowing under water bath, then redissolving by a liquid phase mobile phase and redissolving, taking an supernatant for sample introduction and determining; 2)separating liquid phase: taking an anti-phase silica gel chromatographic column as a separating medium of a liquid phase part of a liquid chromatograph / mass spectrometer, performing isocratic elution by a mobile phase with a fixed ratio after sample introduction, preliminarily separating an interferent, an object to be detected, and the internal standard; wherein a mobile phase A is selected from a formic acid aqueous solution, an acetate aqueous solution, a trifluoroacetic acid aqueous solution or an ammonium acetate aqueous solution, a mobile phase B is selected from acetonitrile or methanol, and the phase A accounts for 30-90% of whole mobile phase; and 3)detecting by mass spectrum: according to set ionizationoun condition, the mass spectrum part of the liquid chromatograph / mass spectrometer employs a SRM scan function for detect the salvianolic acid L in blood plasma and the content of the internal standard.

Description

technical field [0001] The invention relates to a method for the content of medicine in blood plasma, in particular to a method for measuring salvianolic acid L in blood plasma. Background technique [0002] Salvianolic acid L is a new phenolic acid compound discovered by Tianjin Tasly Group Research Institute, which has pharmacological effects such as anti-oxidation, scavenging free radicals, inhibiting platelet aggregation and anti-thrombosis. [0003] Its chemical structural formula is as follows: [0004] [0005] Its molecular weight is as follows: 538 [0006] Its molecular formula is as follows: C 27 h 22 o 12 [0007] The compound and its preparation method are disclosed in Chinese Patent: A New Salvianolic Acid Compound L, Its Preparation Method and Application, CN201010135800.6 [0008] Liquid chromatography-mass spectrometry (HPLC-MS), also known as liquid chromatography-mass spectrometry, uses liquid chromatography as the separation system and mass spect...

Claims

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Application Information

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IPC IPC(8): G01N30/89G01N30/02
Inventor 李伟李淑明王相阳褚扬郭嘉华马晓慧周水平朱永宏
Owner TIANJIN TASLY PHARMA CO LTD
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