Phase chromatography tandem mass spectrum method for NNN optical isomer separation and detection in tobacco

A technology of optical isomers and convergence chromatography, applied in the field of convergence chromatography tandem mass spectrometry, achieves high sensitivity, simple sample pretreatment process, and good repeatability

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

And about ( S )-NNN and ( R )-NNN separation by convergence chromatography or convergence chromatography tandem mass spectrometry has not been reported

Method used

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  • Phase chromatography tandem mass spectrum method for NNN optical isomer separation and detection in tobacco
  • Phase chromatography tandem mass spectrum method for NNN optical isomer separation and detection in tobacco
  • Phase chromatography tandem mass spectrum method for NNN optical isomer separation and detection in tobacco

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example 1

[0024] (1) Instruments and reagents:

[0025] Convergence chromatography tandem mass spectrometer (Waters, USA); ultrasonic instrument (KQ-700DB, Kunshan Ultrasonic Instrument Co., Ltd.).

[0026] Racemic NNN and ( R )-NNN standard (Toronto Research Chemicals, Canada); Methanol (DUKSAN, South Korea, chromatographically pure); Acetic acid (≥99.7%, Fisher Scientific).

[0027] (2) Instrument working conditions:

[0028] The chromatographic conditions and mass spectrometry conditions of the instrument are as described above and will not be repeated here.

[0029] Among them, the selection of chromatographic columns in the chromatographic conditions mainly examines CHIRALPAK® AD-3 chromatographic columns and CHIRALPAK® IG-3 chromatographic columns. on different columns ( S )-NNN and ( R )-NNN The separation results are as follows figure 1 shown. Visible, in view of the excellent separation efficiency of convergence chromatography, ( S )-NNN and ( R )-NNN splits into two c...

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Abstract

The invention relates to a phase chromatography tandem mass spectrum method for N-nitrosonornicotine (NNN) optical isomer separation and detection in tobacco, and belongs to the technical field of tobacco chemistry analysis. A methanol solution containing 0.5% of acetic acid is used for extracting (S)-NNN and (R)-NNN in a tobacco sample, and after the extracting solution is filtered, UPC2-MS / MS isused for analyzing and quantifying the concentration of (S)-NNN and (R)-NNN in the extracting solution. The sample treating process is simple and quick, and batched strict work analysis is convenient. 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 (S)-NNN is 0.21 ng / mL, the quantitation limit is 0.69 ng / mL, the detection limit of (R)-NNN is 0.34 ng / mL, and the quantitation limit is 1.12 ng / mL. The method is high in sensitivity and good in repeatability and is applied to the separation and measurement of the N-nitrosonornicotine optical isomer in the tobacco sample.

Description

technical field [0001] The present invention relates to a kind of tobacco N - A convergence chromatography tandem mass spectrometry method for the separation and determination of nitrosonornicotine (NNN) optical isomers, which belongs to the field of tobacco chemical analysis. Background technique [0002] N -Nitrosonornicotine (NNN) is produced by the nitrosation of the tobacco alkaloid nornicotine during tobacco conditioning and processing. important cause. In its molecular structure, the carbon atom at the 2-position on the tetrahydropyrrole ring has chirality, so NNN has two enantiomers, namely ( S )-NNN and ( R )-NNN. Toxicology research certificate ( S )-NNN is more carcinogenic than ( R )-NNN. Therefore, the separation and determination of NNN enantiomers in tobacco can provide potential references for research on smoking and health, and also provide potential new ideas for research on reducing the harm of cigarettes. [0003] At present, there are few litera...

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 邓惠敏范子彦刘珊珊杨飞李中皓闫丽萍王颖卢鹏金静静边照阳唐纲岭
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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