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A pretreatment method of nitrofuran metabolites

A technology for nitrofuran and metabolites, which is applied in the field of nitrofuran metabolite detection, can solve problems such as long pretreatment process time, and achieve the effects of accelerating derivatization speed, speeding up separation speed, and reducing derivatization time.

Inactive Publication Date: 2019-10-22
深圳市深大检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above existing technical solutions have the following defects: the derivatization process needs to be hydrolyzed at 37°C for 16 hours in the dark, which makes the pretreatment process of nitrofuran metabolites take a long time

Method used

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  • A pretreatment method of nitrofuran metabolites
  • A pretreatment method of nitrofuran metabolites
  • A pretreatment method of nitrofuran metabolites

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The pretreatment method of nitrofuran metabolites comprises the following steps, the following is the preparation of the sample solution to be tested:

[0036] S1: Take a 2g sample (the sample in this example is a pork sample), wash the sample with 5 mL of methanol:water solution with a volume ratio of 2:1, clean the sample, crush the sample to obtain a sample, and add 0.5 ml 0.1 μg / ml four kinds of nitrofuran metabolites mixed internal standard standard solution (diluted with methanol);

[0037] S2: Add 10mL 0.2mol / L hydrochloric acid to the sample and shake well, add 0.3mL 0.05mol / L derivatization reagent (solvent is dimethyl sulfoxide), the derivatization reagent is o-nitrobenzaldehyde, in a light-proof environment Ultrasonic at 50°C for 1h;

[0038] S3: Use 1mol / L sodium hydroxide solution to adjust the pH to 7.4, add 3ml of 1mol / L layer-promoting agent, the layer-promoting agent is sodium chloride solution, dilute to 25ml with water, add 10ml cyclohexane, 1g Neut...

Embodiment 2

[0045] The difference from Example 1 is: in S2, ultrasonication was performed at 60° C. for 1.2 h.

Embodiment 3

[0047] The difference from Example 1 is: in S2, ultrasonication was performed at 65°C for 1.5h,

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Abstract

The invention relates to a pretreatment method of nitrofuran metabolites and belongs to the technical field of detection of the nitrofuran metabolites. The method comprises the following steps: S1) cleaning a sample and stirring the sample to obtain a test sample; S2) adding hydrochloric acid and a derivatization reagent into the test sample, and carrying out ultrasonic treatment for 1-1.5 h under50-65 DEG C; S3) adjusting the PH to 7.4, adding cyclohexane, neutral alumina and a layering promoting agent, and carrying out refrigerated centrifugation after shaking to obtain a bottom solid phase, a middle water phase A and a top organic phase; S4) carrying out solid-phase extraction on the middle water phase A, and then, carrying out eluting through an eluent to obtain eluate B; and S5) carrying out nitrogen drying on the eluate B, and carrying out initial mobile phase volume determination. The method has the effect of shortening the pretreatment time of the nitrofuran metabolites.

Description

technical field [0001] The invention relates to the technical field of detection of nitrofuran metabolites, in particular to a pretreatment method for nitrofuran metabolites. Background technique [0002] At present, nitrofuran drugs are a kind of artificially synthesized broad-spectrum antibiotics. Because of their low price and good effect, they are widely used in livestock, poultry and aquaculture. Because nitrofuran drugs and their metabolites are carcinogenic, Teratogenic side effects. Some countries have banned the use of nitrofuran drugs in livestock, poultry and aquatic animal food. However, the prototype nitrofuran drugs metabolize rapidly in the body and cannot be detected, but their metabolites are bound to proteins. Guaranteed to exist stably for a long time. Therefore, the detection of nitrofuran drug metabolites is generally used as the target analyte to achieve the purpose of detecting nitrofuran drug residues. [0003] There are many existing detection meth...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/14
CPCG01N30/06G01N30/14G01N2030/045G01N2030/062
Inventor 曹荣
Owner 深圳市深大检测有限公司
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