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A high-performance liquid chromatography-tandem mass spectrometry detecting method for a bactericide interception amount in cigarette mainstream smoke

A technology of cigarette mainstream smoke and high-efficiency liquid phase, which is applied in the field of tobacco chemical analysis, can solve the problems that the accuracy needs to be improved, and achieve the effect of improving accuracy

Inactive Publication Date: 2017-07-04
CHINA TOBACCO YUNNAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the common determination methods of fungicides used in tobacco include gas chromatography, liquid chromatography or gas chromatography, gas chromatography electron capture detector and mass spectrometry detection method, gas chromatography flame photometric detection method, liquid chromatography mass spectrometry Usage, etc., but the accuracy of the evaluation needs to be improved

Method used

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  • A high-performance liquid chromatography-tandem mass spectrometry detecting method for a bactericide interception amount in cigarette mainstream smoke
  • A high-performance liquid chromatography-tandem mass spectrometry detecting method for a bactericide interception amount in cigarette mainstream smoke

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Select commercially available domestic cigarette samples, and measure the migration of fungicides in the total particulate matter of mainstream cigarette smoke according to the above test method. The results are shown in Table 1. No fungicide residues such as thiophanate-methyl, carbendazim, propamocarb, and sclerotin were detected in the total particulate matter of mainstream cigarette smoke. Wherein: retention rate of the filter tip (wt%)=(retention amount in the filter tip / residual amount in shredded tobacco before cigarette smoking)×100 wt%.

[0053] Table 1 Detection results of fungicide migration in total particulate matter in mainstream cigarette smoke

[0054]

[0055] Note: / in the table means not detected.

Embodiment 2

[0057] Since the above-mentioned fungicides were not detected in the total particulate matter of the mainstream smoke of commercially available cigarettes, additional injections of different concentrations of fungicides (thiophanate-methyl, carbendazim and propamocarb) were used to inject 1ug / 20 sticks, 4ug / 20 sticks, 20ug / 20 sticks and 80ug / 20 sticks were added to the cigarette sticks. After smoking, the test method was used to measure thiophanate-methyl, carbendazim and propamocarb in the total particulate matter of cigarette mainstream smoke. Determination.

[0058] The results showed that when the amount of thiophanate-methyl added to cigarettes was 1.0ug / 20 and 4.0ug / 20, no thiophanate-methyl and its metabolites were detected in the particulate matter of cigarette mainstream smoke Carbendazim; when the amount of thiophanate-methyl added to cigarettes was 20ug / 20 and 80ug / 20, more trimethylthiophanate and its metabolites were detected in the particulate matter of cigarette...

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Abstract

A high-performance liquid chromatography-tandem mass spectrometry detecting method for a bactericide interception amount in cigarette mainstream smoke is disclosed. The method includes (1) smoking a cigarette, and capturing total granule matters in mainstream smoke by utilizing a Cambridge filter; (2) cutting the Cambridge filter into pieces, then adding the pieces into a centrifuge tube, adding acetonitrile and an internal standard liquid into the centrifuge tube, and vibrating the centrifuge tube to infiltrate the pieces; (3) adding a solid extracting agent into the centrifuge tube, vibrating the centrifuge tube, and performing centrifugal separation; (4) measuring a supernatant liquid to a clean centrifuge tube, vibrating the centrifuge tube, and performing centrifugal separation; and (5) analyzing a supernatant liquid by adopting high-performance liquid chromatography-tandem mass spectrometry, wherein a C<18> high-performance liquid chromatography column is adopted as a chromatography column, the temperature of the column is 25 DEG C, the injection volume is 10 [mu]L, a mobile phase is a gradient mixture consisting of water and acetonitrile, the flow speed is 200 [mu]L / min, positive ion scanning is adopted as a scanning manner, a multiple-reaction monitoring manner is adopted as a monitoring manner, the electrospray voltage is 5500 V, the pressure of atomized gas is 0.414 MPa, and the temperature of an ion source is 500 DEG C.

Description

technical field [0001] The invention belongs to the technical field of tobacco chemical analysis, and specifically provides a high performance liquid phase-tandem mass spectrometry detection method for the interception amount of fungicides in mainstream smoke of cigarettes. Background technique [0002] Fungicides are a class of pesticides used to prevent and control plant diseases caused by various pathogenic microorganisms, generally referring to fungicides. However, internationally, it is usually used as a general term for agents to prevent and control various pathogenic microorganisms. From the perspective of controlling crop diseases, fungicides are currently irreplaceable by other substances, and the overall demand for fungicides continues to increase. The global growth rate of fungicides has reached nearly 8%, and triazole fungicides will still be the protagonists. In order to prevent tobacco leaves from being engulfed by diseases and insect pests and ensure the yiel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 李雪梅曾婉俐宋春满高茜管莹田丽梅向明
Owner CHINA TOBACCO YUNNAN IND