Method for analyzing chiral drug enantiomers in biological body fluid through column-switching liquid chromatography

A liquid chromatography analysis and chiral drug technology, which is applied in the field of column switching-liquid chromatography analysis of chiral drug enantiomers in biological fluids, can solve the problems of time-consuming, solvent-consuming, large sample loss, etc., and achieves reduction of cumbersome steps, improve the degree of automation, and the effect of sensitive online detection

Active Publication Date: 2014-01-01
中国人民解放军联勤保障部队第九四〇医院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The matrix components in biological fluids are complex, and the concentration of a single enantiomer is low. There are a series of problems in the analysis and determination, such as complex and cumbersome sample pretreatment steps, large sample loss, low recovery rate and accuracy of the method, time-consuming, and solvent-consuming. Therefore, It is necessary to establish a rapid, sensitive and accurate method for single enantiomer analysis in biological fluids

Method used

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  • Method for analyzing chiral drug enantiomers in biological body fluid through column-switching liquid chromatography
  • Method for analyzing chiral drug enantiomers in biological body fluid through column-switching liquid chromatography
  • Method for analyzing chiral drug enantiomers in biological body fluid through column-switching liquid chromatography

Examples

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Effect test

Embodiment 1

[0030] Example 1 The method for column switching-liquid chromatography analysis of chiral drug enantiomers in biological fluids comprises the following steps:

[0031] (1) Dissolve the standard substance of chiral drug racemate - propranolol hydrochloride racemate standard substance at a temperature of 20°C with absolute ethanol to make a standard solution with a concentration of 5mg / mL; the standard solution Use blank plasma at a temperature of 20°C (see figure 1 ) was diluted to make a plasma sample with a concentration of 0.5 mg / mL.

[0032] (2) Put the plasma sample in a 1.5mL centrifuge tube with a stopper, centrifuge at a speed of 4000r / min for 5min, carefully draw the supernatant and place it in a centrifuge tube for sample injection.

[0033] (3) Preparation of limited-access packing column: the outer surface of silica gel with a particle size of 5 μm is bonded with hydrophilic polyvinyl alcohol, and the inner surface is bonded with non-polar hexylamine to form a colu...

Embodiment 2

[0041] Example 2 The method for column switching-liquid chromatography analysis of chiral drug enantiomers in biological fluids, comprising the following steps:

[0042] (1) Dissolve the standard substance of chiral drug racemate - the standard substance of propranolol hydrochloride racemate at a temperature of 30°C with absolute ethanol to make a standard solution with a concentration of 4mg / mL; the standard solution Use blank plasma at a temperature of 30°C (see image 3 ) was diluted to make a plasma sample with a concentration of 1.5 mg / mL.

[0043] (2) Put the plasma sample in a 2.0mL centrifuge tube with a stopper, centrifuge at a speed of 2000r / min for 3min, carefully draw the supernatant and place it in a centrifuge tube for sample injection.

[0044] (3) Preparation of limited-access packing column: the outer surface of silica gel with a particle size of 5 μm is bonded with hydrophilic polyvinyl alcohol, and the inner surface is bonded with non-polar hexylamine to fo...

Embodiment 3

[0052] Example 3 A method for column switching-liquid chromatography analysis of chiral drug enantiomers in biological fluids, comprising the following steps:

[0053] (1) Dissolve the standard substance of chiral drug racemate - propranolol hydrochloride racemate standard substance with absolute ethanol at a temperature of 5°C to make a standard solution with a concentration of 4.5mg / mL; The solution was diluted with blank plasma at a temperature of 5°C to prepare a plasma sample with a concentration of 1.0 mg / mL.

[0054] (2) Put the plasma sample in a 1mL centrifuge tube with a stopper, centrifuge at a speed of 1000r / min for 10min, carefully draw the supernatant and place it in a centrifuge tube for sample injection.

[0055] (3) Preparation of limited-access packing column: the outer surface of silica gel with a particle size of 5 μm is bonded with hydrophilic polyvinyl alcohol, and the inner surface is bonded with non-polar hexylamine to form a column with an inner diamet...

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Abstract

The invention relates to a method for analyzing chiral drug enantiomers in biological body fluid through column-switching liquid chromatography, which comprises the following steps: (1) preparing a chiral drug racemate standard product into a standard solution having a certain concentration; and diluting the standard solution into a plasma sample having a certain concentration; (2) centrifuging the plasma sample, and taking the supernate as an injected sample for later use; (3) preparing a restricted-access material column; (4) preparing a chiral fixed phase; (5) putting the restricted-access material column used as a pretreatment column and the chiral fixed phase used as an analytical column into a column-switching restricted-access material-chiral fixed phase high performance liquid chromatography system; and (6) injecting the supernate of the plasma sample into a sampler in the column-switching restricted-access material-chiral fixed phase high performance liquid chromatography system; and by using borate buffer-methanol or water-methanol as a mobile phase of the pretreatment column, separating with borate buffer-isopropanol-anhydrous alcohol to obtain a chromatogram of different single enantiomers having different appearance times. The invention has the characteristics of high speed, high convenience and high sensitivity.

Description

technical field [0001] The invention relates to the application of column switching technology and the field of chiral drug enantiomers, in particular to a column switching-liquid chromatography method for analyzing chiral drug enantiomers in biological fluids. Background technique [0002] From several drug injury incidents that shocked the world in the last century, people have gradually realized that the slight differences in the three-dimensional configurations between the enantiomers of chiral drugs lead to differences in their pharmacological activity, metabolic process and toxicity in the human body. Significant differences exist. With the continuous development of science and technology, more in-depth in vivo studies on single enantiomers of chiral drugs are carried out. The development of single enantiomer new drugs is of great significance. [0003] The physical and chemical properties of the enantiomers of chiral drugs are similar, only the optical rotation is d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/20
Inventor 贾正平王荣谢华武晓玉张娟红
Owner 中国人民解放军联勤保障部队第九四〇医院
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