Phase chromatography tandem mass spectrum measuring method for NNK and NNN in tobacco

A determination method and tandem mass spectrometry technology, which can be applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of convergence chromatography or convergence chromatography tandem mass spectrometry and other problems that have not been reported, and achieve a simple and repeatable sample pretreatment process. , the effect of high sensitivity

Active Publication Date: 2018-09-14
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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Problems solved by technology

[0003] At present, the determination methods of NNK and NNN mainly include gas chromatography, gas chromatography-mass spectrometry, liquid chromatography and liquid chromatography-tandem mass spectrometry. There are no reports on the convergence chromatography or convergence chromatography-tandem mass spectrometry for the determination of NNK and NNN.

Method used

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  • Phase chromatography tandem mass spectrum measuring method for NNK and NNN in tobacco
  • Phase chromatography tandem mass spectrum measuring method for NNK and NNN in tobacco
  • Phase chromatography tandem mass spectrum measuring method for NNK and NNN in tobacco

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example 1

[0025] (1) Instruments and reagents:

[0026] Convergence chromatography tandem mass spectrometer (Waters, USA); ultrasonic instrument (KQ-700DB, Kunshan Ultrasonic Instrument Co., Ltd.); HY-8 speed-adjustable oscillator (Changzhou Guohua Electric Co., Ltd.).

[0027] NNK and NNN standards (Toronto Research Chemicals, Canada); Methanol (DUKSAN, South Korea, chromatographically pure); Acetic acid (≥99.7%, Fisher Scientific).

[0028] (2) Instrument working conditions:

[0029] The chromatographic conditions and mass spectrometry conditions of the instrument are as described above and will not be repeated here.

[0030] Among them, the selection of chromatographic columns in the chromatographic conditions mainly examines the ACQUITY UPC 2 CSH Fluoro Phenyl Columns, ACQUITY UPC 2 HSS C18 column, ACQUITY UPC 2 BEH Columns and ACQUITY UPC 2 BEH 2EP column. The separation results of NNK and NNN standards on different chromatographic columns are as follows: figure 1 shown....

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Abstract

The invention relates to a phase chromatography tandem mass spectrum measuring method for 4-(methyl nitrosamino)-1-(3-pyridyl)-1-butanone(NNK) and N-nitrosonornicotine (NNN) in tobacco, and belongs tothe technical field of tobacco chemistry analysis. A methanol solution containing 0.5% of acetic acid is used for extracting NNK and NNN in a tobacco sample, and after the extracting solution is filtered, UPC2-MS/MS is used for analyzing and quantifying the concentration of NNK and NNN in the extracting solution. The sample treating process is simple and quick, and batched strict work analysis isconvenient. When the phase chromatography tandem mass spectrum is used for detection, the used main moving phase is supercutical fluid CO2, a small amount of methyl alcohol is used as a cosolvent, and the environmentally friendly advantage is achieved. According to the method, the detection limit of NNK is 0.05 ng/mL, the quantitation limit is 0.18 ng/mL, the detection limit of NNN is 0.04 ng/mL,and the quantitation limit is 0.12 ng/mL. The method is high in sensitivity and good in repeatability and is applied to synchronous measurement of NNK and NNN in the tobacco sample.

Description

technical field [0001] The invention relates to 4-(methylnitrosamine)-1-(3-pyridyl)-1-butanone (NNK) and N - A method for determining nitrosonornicotine (NNN) by convergence chromatography tandem mass spectrometry, which belongs to the field of tobacco chemical analysis. Background technique [0002] Tobacco-specific nitrosamines are tobacco-specific compounds. At present, people pay more attention to 4 kinds of nitrosamines with high content, namely 4-(methylnitroso)-1-(3-pyridyl)-1-butanol Ketones (NNK), N - Nitrosonornicotine (NNN), N - Nitrosobasine (NAB) and N - Nitrosoanatabine (NAT). Among them, NNK and NNN are listed as Class 1 carcinogens (carcinogenic to humans) by the National Cancer Research Institute (IARC), and NAB and NAT are listed as Class 3 carcinogens (suspected carcinogens). In addition, in view of the carcinogenicity of NNK and NNN, NNK and NNN were included in the list of harmful and potentially harmful components of tobacco products and smoke rele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 邓惠敏刘珊珊范子彦金静静杨飞李中皓卢鹏王颖边照阳唐纲岭
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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