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Method for detecting sec-butylamine residue and application of method

A technology of sec-butylamine and hyphenated instrument, which is applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of unsuitable practical application, single substrate, complicated processing steps, etc., and achieves less consumables, low recovery rate, and processing method. cumbersome effect

Active Publication Date: 2017-05-10
QINGDAO HARWARS BIOLOGY GRP LTD
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AI Technical Summary

Problems solved by technology

[0002] At present, gas phase or ultraviolet detection methods are mostly used for the detection of sec-butylamine. This method is prone to false positives, and the pre-treatment steps are cumbersome, with low recovery and poor stability. It is not suitable for practical application due to the single matrix.

Method used

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  • Method for detecting sec-butylamine residue and application of method
  • Method for detecting sec-butylamine residue and application of method
  • Method for detecting sec-butylamine residue and application of method

Examples

Experimental program
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Embodiment

[0024] 1. Preparation of standard solution

[0025] 1.1 Preparation of stock solution

[0026] Accurately weigh 10.00mg of sec-butylamine and dissolve it in ultrapure water, dilute to 10mL, use it as a stock solution of 1000μg / mL (the actual concentration should be multiplied by the purity of sec-butylamine), and store in refrigerated storage at 4°C;

[0027] 1.2 Preparation of working solution

[0028] Accurately pipette 1mL of 100μg / mL sec-butylamine stock solution into a 50mL centrifuge tube, add 1mL of 80% methanol aqueous solution and 2mL of carbonate buffer solution with pH 9.8, add 1mL of 50g / L dansyl chloride acetone solution, at 50℃ Shake in a water bath for 1 hour, after cooling, dilute to 10 mL with methanol, centrifuge at 4000 r / min for 5 minutes, and filter the membrane to obtain 10 ppm working solution.

[0029] 1.3 Preparation of standard working curve

[0030] Prepare 5, 10, 20, 50, 100 ng / mL standard solutions (constant volume with 80% methanol aqueous solu...

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Abstract

The invention discloses a method for detecting sec-butylamine residue and belongs to the technical field of medicine detection. The method comprises: using methanol solution to extract sec-butylamine in a sample, subjecting carbonate buffer solution and dansyl chloride acetone solution to derivatization, and detecting with high-performance liquid chromatography-tandem mass spectrometry apparatus; the methanol has a concentration of 80%. The method has the advantages that the derivatization of carbonate buffer solution and dansyl chloride acetone solution helps purify sec-butylamine; liquid-mass detection for sec-butylamine residue is reforming progress, the detection is sensitive and high in performance, and the detection limit is low; the methanol solution is used as an extracting solvent, material consumption is low, and the cost is saved.

Description

technical field [0001] The invention belongs to the field of pesticide residue detection, and in particular relates to a method and application for detecting sec-butylamine residue. Background technique [0002] At present, gas phase or ultraviolet detection methods are mostly used for the detection of sec-butylamine. This method is prone to false positives, and the pre-treatment steps are cumbersome, with low recovery rate and poor stability. It is not suitable for practical application due to its single matrix. Contents of the invention [0003] In order to solve the problems in the prior art, the technical solution of the present invention is: [0004] A method for detecting residual sec-butylamine, using methanol aqueous solution to extract sec-butylamine in the sample, derivatizing with carbonate buffer solution and dansyl chloride acetone solution, and then using high performance liquid chromatography mass spectrometry for detection; the methanol solution The concen...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/14
CPCG01N30/02G01N30/14G01N2030/062G01N2030/067
Inventor 刘刚韩肖周凯陈雷
Owner QINGDAO HARWARS BIOLOGY GRP LTD
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