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Method for analyzing pesticide residues in tobacco via heart-cutting two-dimensional chromatography-mass spectrometry combination

A two-dimensional chromatographic and heart-cutting technology, which is applied in the field of pesticide residue analysis in tobacco, can solve the problems of obvious matrix inhibition effect, difficult matrix removal, and affecting analysis accuracy and repeatability.

Inactive Publication Date: 2019-01-11
SHANGHAI TOBACCO GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the detection process of tobacco pesticide residues, some macromolecular proteins and some non-polar substance sub-matrix are difficult to remove, and the matrix inhibition effect is more obvious, which affects the accuracy and repeatability of the analysis.

Method used

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  • Method for analyzing pesticide residues in tobacco via heart-cutting two-dimensional chromatography-mass spectrometry combination
  • Method for analyzing pesticide residues in tobacco via heart-cutting two-dimensional chromatography-mass spectrometry combination
  • Method for analyzing pesticide residues in tobacco via heart-cutting two-dimensional chromatography-mass spectrometry combination

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0130] 1. Sample pretreatment

[0131] Take a certain amount of tobacco powder sample, add pure water and oscillate until the sample is fully infiltrated by water and then let it stand for 8-12 minutes. The ratio of the mass g of tobacco added to the volume mL of water added is 2:5-15. Then add the internal standard solution, place in a vortex shaker and vibrate at 1500-2500r / min for 0.8-1.2min. The internal standard solution is an acetonitrile solution containing an internal standard sample, the concentration of the internal standard sample in the internal standard solution is 100ng / mL, and the ratio of the mass g of tobacco added to the volume mL of the internal standard solution is 2:5-15.

[0132] Then add the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) kit powder package, place in a vortex shaker at 1500-2500r / min for 1.8-2.2min, and then centrifuge at 4500-5500r / min for 9 -11min, take the first supernatant. The powder pack of the kit includes anhydrous magne...

Embodiment 2

[0162] 1. Sample pretreatment

[0163] 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 the internal standard solution, place in a vortex shaker and vibrate at 2000r / min for 1.0min. The internal standard solution is an acetonitrile solution containing an internal standard sample, and the concentration of the internal standard sample in the internal standard solution is 100 ng / mL.

[0164] Then add the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) kit powder package, place in a vortex shaker at 2000r / min for 2.0min, then centrifuge at 5000r / min for 10min, and take the first supernatant liquid. The powder pack of the kit includes 4g of anhydrous magnesium sulfate, 1g of sodium chloride and 0.5g of sodium bicitrate.

[0165] Put 1mL of the first supernatant into the small tube containing the adsorbent of the QuEChERS kit, oscillate with...

Embodiment 3

[0194] As shown in 2 in the above-mentioned embodiment 2, accurately pipette the standard samples of 74 kinds of pesticide residue components respectively, add the internal standard sample, then add acetonitrile to constant volume, and make a series of mixed standard solutions, wherein the concentration of the internal standard sample is 100ng / mL.

[0195] A series of mixed standard solutions with different concentrations prepared above were detected by heart-cutting two-dimensional chromatography-mass spectrometry system respectively, and the ordinate (Y axis), the mass concentration ratio of its 74 kinds of pesticide residues 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. In the linear concentration range of 10-500ng / mL, The correlation coefficient R of the regression equation of 74 kinds of pesticide residues is greater than 0.99, which has a ...

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Abstract

The invention provides a method for analyzing pesticide residues in tobacco via heart-cutting two-dimensional chromatography-mass spectrometry combination. Sample pretreatment is carried out on the tobacco, and qualitative and quantitative analysis is carried out on a sample to be tested obtained by the pretreatment by adopting a heart-cutting two-dimensional chromatography-mass spectrometry combined system, wherein the heart-cutting two-dimensional chromatography-mass spectrometry combined system comprises a first-dimensional chromatographic column, a current divider, a loop, a two-dimensional chromatographic column and a mass spectrometer which are orderly connected with each other along a sample injection method. The invention further provides the heart-cutting two-dimensional chromatography-mass spectrometry combined system and a use method thereof. The method for analyzing the pesticide residues in the tobacco via the heart-cutting two-dimensional chromatography-mass spectrometrycombination provided by the invention can effectively purify and remove macromolecular interfering substances, maintain the repeatability, stability and accuracy of large-scale sample pesticide residues, especially large sample-size pesticide residue test, and can be used for long-term, large sample amount and multi-component analysis and detection of tobacco pesticide residues.

Description

technical field [0001] The invention belongs to the technical field of analysis of pesticide residues in tobacco, and relates to a method for analyzing pesticide residues in tobacco by heart-cutting two-dimensional chromatography-mass spectrometry, in particular to a method using heart-cutting first-dimensional size exclusion liquid chromatography and second-dimensional size exclusion liquid chromatography. Multidimensional chromatography / tandem mass spectrometry combined with reversed-phase liquid chromatography for the analysis of various pesticide residues in tobacco. 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, and the determination of pesticide residues has always been a research hotspot. The commonly used methods for tobacco pesticide residues mainly include GC-MS / MS and LC-MS / ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/045
Inventor 陈敏吴达戚大伟刘百战
Owner SHANGHAI TOBACCO GRP CO LTD
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