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Method for analyzing carbaryl pesticide residue in tobacco by using combination of central cut two-dimensional liquid chromatogram and mass spectrum

A two-dimensional liquid chromatography and heart-cutting technology, applied in the field of analysis of pesticide residues in tobacco, can solve problems such as cumbersome process, method accuracy and repeatability impact

Inactive Publication Date: 2019-07-19
SHANGHAI TOBACCO GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the pretreatment process is cumbersome, which affects the accuracy and repeatability of the method.

Method used

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  • Method for analyzing carbaryl pesticide residue in tobacco by using combination of central cut two-dimensional liquid chromatogram and mass spectrum
  • Method for analyzing carbaryl pesticide residue in tobacco by using combination of central cut two-dimensional liquid chromatogram and mass spectrum
  • Method for analyzing carbaryl pesticide residue in tobacco by using combination of central cut two-dimensional liquid chromatogram and mass spectrum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0186] 1. Sample pretreatment

[0187] Take 2.000g of tobacco powder sample in a 50mL centrifuge tube, add 10mL of pure water and shake until the sample is fully infiltrated by water, then let it stand for 10min. Then add 10 mL of acetonitrile solution containing the internal standard sample concentration of 100 ng / mL to the centrifuge tube, place in a vortex shaker and vibrate at 2000 r / min for 1.0 min. The internal standard sample is phenyl triphosphate (TPP).

[0188] Then add a powder bag containing 4g of anhydrous magnesium sulfate, 1g of sodium chloride and 0.5g of sodium bicitrate, place it in a vortex oscillator at 2000r / min for 2.0min, then centrifuge at 5000r / min for 10min, take the Serum. The mass ratio of anhydrous magnesium sulfate, sodium chloride, sodium bicitrate and tobacco added is 4:1:0.5:2.

[0189] The sample to be tested was obtained after filtering the supernatant with a 0.22 μm organic phase filter.

[0190] 2. Preparation of standard solution

[0...

Embodiment 2

[0229] As shown in step 2 in the above-mentioned embodiment 1, accurately pipette the standard sample of carbaryl pesticide residues respectively, add the internal standard sample, then add acetonitrile to constant volume, and make a series of standard solutions, wherein the concentration of the internal standard sample is 100ng / mL.

[0230] A series of standard solutions with different concentrations prepared above were respectively detected by a heart-cutting two-dimensional chromatography-mass spectrometry system, and the secondary selected ion peak area ratio of carbaryl residues and corresponding internal standards was taken as the ordinate (Y axis), the mass concentration ratio of its carbaryl residue and the corresponding internal standard substance is the abscissa (X axis), and regression analysis is carried out to obtain a good linear relationship of the regression equation, within the linear concentration range of 2.5~500ng / mL , the correlation coefficient R of the r...

Embodiment 3

[0235] Take the recovery rate, intra-day repeatability, and day-time repeatability of the same tobacco sample investigation method, that is, select a known carbaryl component concentration sample, add a standard solution of known concentration, and then carry out the pretreatment of step 1 in the above-mentioned embodiment 1 , and a heart-cutting two-dimensional chromatography-mass spectrometry system analysis was performed to calculate the recovery rate. At the same time, the same sample solution to be tested was measured in parallel 5 times (n=5) within 1 day and during the day to obtain the precision measurement data of carbaryl pesticide residues. The results are shown in Table 4.

[0236] As can be seen from Table 4, the recovery rate of the target method is between 92.8% and 106.2%, the relative standard deviation (RSD) of intraday repeatability is within 3.1%, and the relative standard deviation (RSD) of daytime repeatability is 5.7%. It shows that the method of the pre...

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Abstract

The invention provides a method for analyzing a carbaryl pesticide residue in tobacco by using the combination of central cut two-dimensional liquid chromatogram and mass spectrum. The method comprises the steps of performing sample pretreatment on the tobacco to acquire a sample to be tested, and using a central cut two-dimensional liquid chromatogram and mass spectrum combined system to test thecarbaryl pesticide residue in the sample to be tested. The method for analyzing the carbaryl pesticide residue in the tobacco by using the combination of the central cut two-dimensional liquid chromatogram and mass spectrum provided by the invention, the pretreatment step is simple, the interference substances in the sample are effectively removed, the ion source pollution is reduced, the pesticide residue detection limit is improved, and thus the method is particularly suitable for improving the test repeatability and accuracy of the carbaryl in many samples.

Description

technical field [0001] The invention belongs to the technical field of pesticide residue analysis in tobacco, and relates to a method for analyzing carbaryl pesticide residues in tobacco by heart-cutting two-dimensional liquid chromatography mass spectrometry. Background technique [0002] As the most widely planted non-food crop in the world, tobacco is grown in 129 countries and regions around the world. Therefore, pesticide residues are an important part of tobacco quality and safety issues. In the list of carcinogens published by the International Agency for Research on Cancer of the World Health Organization, carbaryl exists in three types of carcinogens. The structure of carbaryl is as follows: [0003] [0004] At present, the commonly used methods for tobacco pesticide residues mainly include GC-MS / MS and LC-MS / MS methods. The interference of the matrix has always been an important problem in the accurate determination of pesticide residues. The existing technolo...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/045G01N2030/062
Inventor 陈敏董惠忠吴达刘百战
Owner SHANGHAI TOBACCO GRP CO LTD
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