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Method for determining gamma-hydroxybutyric acid in urine liquid through ion exclusion-ion exchange column switching combined use

A technology of ion exchange column and hydroxybutyric acid, which is applied in the field of determination of γ-hydroxybutyric acid in urine by ion exclusion-ion exchange column switching method, can solve the problems of cumbersome, complicated operation and low recovery rate, and achieve simplification Operation steps, broad application prospects, simple and reliable results

Inactive Publication Date: 2017-08-04
南京市公安局刑事侦查局
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the GC, GC-MS, LC, LC-MS method that the present invention measures gamma-hydroxybutyric acid in the urine and all needs to carry out pretreatment to urine (GHB carries out esterification under strong acid condition to generate GBL and then use organic solvent to extract it for instrument testing), complex operation, cumbersome, and low recovery; develop an ion exclusion-ion exchange column switching method to directly determine gamma-hydroxybutyric acid in urine, and urine does not need ester can be directly detected by ion chromatography

Method used

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  • Method for determining gamma-hydroxybutyric acid in urine liquid through ion exclusion-ion exchange column switching combined use
  • Method for determining gamma-hydroxybutyric acid in urine liquid through ion exclusion-ion exchange column switching combined use
  • Method for determining gamma-hydroxybutyric acid in urine liquid through ion exclusion-ion exchange column switching combined use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: The ion chromatography analysis and detection steps of gamma-hydroxybutyric acid in urine are:

[0031] 1. Pass the urine to be tested through a nylon filter head to remove solid particles; add 1% sodium fluoride after sampling the urine, store it in the refrigerator at 4°C, and analyze it within 24 hours; take volunteers (male, 30 Aged) Urine 10mL in a 15mL centrifuge tube, add 2mL acetonitrile, vortex shake for 3min; put in a centrifuge and centrifuge at 7830rpm for 10min; take the supernatant, nitrogen blowing method to remove acetonitrile; then use 0.22μm nylon water-based membrane Samples were injected directly after removal of solid particles by filtration.

[0032] 2. First, γ-hydroxybutyric acid was separated from other anions in urine by ion exclusion method, and the eluent was 0.2mM heptafluorobutyric acid; inhibition of conductivity detection (tetramethylammonium hydroxide pentahydrate aqueous solution was used to inhibit ), the system temperat...

Embodiment 2

[0035] Embodiment 2: with reference to the method and steps of embodiment 1

[0036] 1. Pass the urine to be tested through a nylon filter head to remove solid particles;

[0037] 2. Separate gamma-hydroxybutyric acid from other anions in urine by ion exclusion method, the eluent is 0.1mM heptafluorobutyric acid; inhibit conductivity detection (tetramethylammonium hydroxide pentahydrate aqueous solution is used to inhibit ), the system temperature is 15°C, and the flow rate is 1.5mL / min;

[0038] 3. Separation of γ-hydroxybutyric acid and heptafluorobutyric acid by column switching ion exchange method, the eluent is 1mM sodium hydroxide; to suppress conductivity detection, the system temperature is 15°C, and the flow rate is 1.5mL / min;

[0039] 4. The result is consistent with Example 1.

Embodiment 3

[0040] Embodiment 3: with reference to the method and steps of embodiment 1

[0041] 1. Pass the urine to be tested through a nylon filter head to remove solid particles;

[0042] 2. First, γ-hydroxybutyric acid was separated from other anions in urine by ion exclusion method, and the eluent was 0.4mM heptafluorobutyric acid; ), the system temperature is 15°C, and the flow rate is 2.0mL / min;

[0043] 3. Separation of γ-hydroxybutyric acid and heptafluorobutyric acid by column switching ion exchange method, the eluent is 1.0mM sodium hydroxide; to suppress conductivity detection, the system temperature is 15°C, and the flow rate is 2.0mL / min;

[0044] 4. The result is consistent with Example 1.

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Abstract

The invention provides a method for determining gamma-hydroxybutyric acid in urine liquid through ion exclusion-ion exchange column switching combined use. According to the method, firstly, by using an ion exclusion method, strong negative ions in the urine liquid are separated from the gamma-hydroxybutyric acid; then, by using a column switching iron exchange method, the gamma-hydroxybutyric acid is separated from heptafluorobutyric acid; the fast and standard detection of the gamma-hydroxybutyric acid in the urine liquid is realized by using an ion exclusion-ion exchange column switching combined use method. Compared with the existing gas chromatography-mass spectrometry combined use method, an ion chromatography method has the advantages that the esterification pretreatment on the urine liquid is not needed; direct sampling can be performed; the speed is high; the operation is simple; the sensitivity is high.

Description

technical field [0001] The invention relates to a method for determining gamma-hydroxybutyric acid in urine by an ion exclusion-ion exchange column switching method. Background technique [0002] γ-hydroxybutanoic acid, also known as 4-hydroxybutanoic acid (4-Hydroxybutanoic acid), or GHB, is a central nervous system depressant. It has strong sedative and amnestic effects and is favored by criminals. The phenomenon of abuse is becoming more and more serious , such as being used for rape etc., bring serious social problems. Therefore, γ-hydroxybutyrate is recognized as a drug in many countries. Gamma-hydroxybutyrate has historically been used as a common sedative for insomnia, depression, narcolepsy, and alcoholism, and to enhance athletic performance; in practice, gamma-hydroxybutyrate is often used potassium or sodium salt. Gamma-hydroxybutyric acid, a naturally occurring substance found in the central nervous system, is also present in wine, beef, citrus fruits, and in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/60
CPCG01N30/6039
Inventor 王勇刘军伟朱岩
Owner 南京市公安局刑事侦查局
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