Method for determining tobacco-specific nitrosamines in cigarette mainstream smoke by employing online two-dimensional chromatography-tandem mass spectrometry

A cigarette mainstream smoke and two-dimensional chromatography technology, applied in the field of chemical composition analysis in tobacco, can solve the problems of matrix interference, difficulty in accurate quantification, low nitrosamine content, etc.

Inactive Publication Date: 2020-01-03
SHANGHAI TOBACCO GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In view of the shortcomings of the prior art described above, the purpose of the present invention is to provide an online two-dimensional chromatography tandem mass spectrometry method for the determination of tobacco-specific nitrosamines in cigarette mainstream smoke, which can effectively solve the problem of tobacco-specific nitrosamines in cigarette smoke. Low amine content, serious matrix interference, and difficult to quantify accurately, especially suitable for the accurate determination of trace nitrosamines in the smoke of medium and small cigarettes

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  • Method for determining tobacco-specific nitrosamines in cigarette mainstream smoke by employing online two-dimensional chromatography-tandem mass spectrometry
  • Method for determining tobacco-specific nitrosamines in cigarette mainstream smoke by employing online two-dimensional chromatography-tandem mass spectrometry
  • Method for determining tobacco-specific nitrosamines in cigarette mainstream smoke by employing online two-dimensional chromatography-tandem mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0145] 1. Sample pretreatment

[0146] Select 20 cigarettes, and use the filter to capture the cigarette smoke after lighting. Specifically, use a 20-hole rotary disc smoking machine to suck the cigarettes, and collect the smoke according to the method specified in ISO 3308:2000 to make the smoke adsorb On a Cambridge filter disc with a diameter of 92mm. Put the Cambridge filter in a 100mL Erlenmeyer flask, add 20mL of 0.1mol / L ammonium acetate aqueous solution and 100μL of internal standard solution, place it in a vortex mixing oscillator and extract for 30min, then take the extract and pass it through a 0.22μm PTFE filter membrane to obtain the sample solution. The internal standard solution is NNN-d 4 、NNK-d 4 , NAT-d 4 、NAB-d 4 Methanol solution, NNN-d in internal standard solution 4 、NNK-d 4 , NAT-d 4 、NAB-d 4 The concentration was 2 μg / mL.

[0147] 2. Qualitative and quantitative analysis

[0148] Pipette 0.1 mL of NNN, NNK, NAT, and NAB standard substances wi...

Embodiment 2

[0172] As shown in step 2 in the above example 1, accurately pipette the stock solution, add 50 μL internal standard solution, and dilute to the mark with 0.1mol / L ammonium acetate aqueous solution to prepare a series of concentrations of 0.1, 0.2, 0.5, 1, 2, 5, 10, 20, 100ng / mL standard solution, the internal standard concentration is 10ng / mL.

[0173] A series of standard solutions with different concentrations prepared above were analyzed by UPCC-HPLC-MS / MS respectively, and the chromatographic peak area ratios of the 4 kinds of nitrosamine components and the internal standard were taken as the ordinate (Y axis), and the corresponding nitrosamines The concentration ratio of the components and the internal standard is the abscissa (X-axis), and regression analysis is performed to obtain a good linear relationship of the regression equation. Within the linear concentration range of 0.1 to 100ng / mL, the correlation coefficients of the regression equations of the four nitrosamin...

Embodiment 3

[0177] A slim cigarette sample was selected as the object, and the inter-day repeatability, intra-day repeatability, recovery rate and detection limit of the method were investigated. As in the pretreatment and analysis process in the above-mentioned Example 1, the samples were measured in parallel 9 times under the same conditions within one day and during the day, and the repeatability of the method was investigated by the relative standard deviation of the measurement results. The standard solutions of high, medium and low concentrations of TSNAs were added to the extraction process of the slim cigarette smoke samples, and the recoveries of different concentrations of standard addition were calculated. At the same time, internal standards of different concentrations were added to the extraction process of the slim cigarette smoke sample, and the 10-fold signal-to-noise ratio was used as the limit of quantification (LOQ) of the method. The specific data are shown in Table 3. ...

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Abstract

The invention provides a method for determining tobacco-specific nitrosamines in cigarette mainstream smoke by employing online two-dimensional chromatography-tandem mass spectrometry. The method comprises the steps of capturing and extracting cigarette mainstream smoke and then obtaining a sample solution; and carrying out qualitative and quantitative analysis on a nitrosamine component in the sample solution by adopting ultrahigh performance bonded-phased chromatography-liquid chromatography-mass spectrometry (UPCC-HPLC-MS / MS). The invention further provides an online two-dimensional chromatography-tandem mass spectrometry system for the tobacco-specific nitrosamines in the cigarette mainstream smoke and an application method of the online two-dimensional chromatography-tandem mass spectrometry system. The method for determining the tobacco-specific nitrosamines in the cigarette mainstream smoke by employing the online two-dimensional chromatography-tandem mass spectrometry providedby the invention has the advantages of being simple in operation, fast in detection and high in sensitivity and is suitable for routine analysis and detection of the tobacco-specific nitrosamines in the cigarette mainstream smoke, especially accurate quantification of traces of nitrosamines in medium and thin cigarette smoke samples.

Description

technical field [0001] The invention belongs to the technical field of chemical component analysis in tobacco, and relates to an online two-dimensional chromatography-tandem mass spectrometry method for determining tobacco-specific nitrosamines in mainstream smoke of cigarettes, in particular to the use of ultra-high performance convergence chromatography-liquid chromatography-mass spectrometry A combined method (UPCC-HPLC-MS / MS) for the determination of tobacco-specific nitrosamines in mainstream cigarette smoke. Background technique [0002] Tobacco-specific nitrosamines (TSNAs) include 4-(N-methylnitrosamine)-1-(3-pyrazyl)-1-butanone (NNK), N-nitrosonornicotine (NNN ), N-nitrosopsine (NAB) and nitrosoanenicotine (NAT), are a class of tobacco-specific harmful substances in tobacco products and smoke, because of their strong carcinogenicity has always been Tobacco researchers at home and abroad are the focus of attention. Accurate determination of the content of tobacco-sp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/20G01N30/36G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/36G01N30/72G01N30/20G01N2030/045G01N2030/062G01N2030/201
Inventor 周妍戚大伟罗辰费婷吴达
Owner SHANGHAI TOBACCO GRP CO LTD
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