Method for determinating nornicotine enantiomer content of smoke-free tobacco product by combined phase chromatography-tandem mass spectrometry

Abstract

The invention discloses a method for determinating the nornicotine enantiomer content of a smoke-free tobacco product by a combined phase chromatography-tandem mass spectrometry. The method is characterized by comprising the following steps: drying, crushing and sieving a smoke-free tobacco product sample, infiltrating the sample by using a sodium hydroxide solution, extracting by using dichloromethane, purifying an extract through matrix solid-phase dispersion extraction, analyzing by two tandem chiral columns-combined phase chromatography-tandem mass spectrometry, and quantitatively detecting a ratio of S-nornicotine to R-nornicotine in the smoke-free tobacco product by a peak area normalization method. According to the method provided by the invention, the sample extracting and purifying method is simple and efficient, pollution of sample liquid to the chromatographic columns can be reduced, the combined phase chromatography-tandem mass spectrometry detection method is high in sensitivity and good in specificity, false positive can be excluded, the analysis time is short, and chiral analysis on the nornicotine in a large batch of smoke-free tobacco product samples can be met.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical analysis, and in particular relates to a method for determining the content of nornicotine enantiomers in smokeless tobacco products by phase convergence chromatography-tandem mass spectrometry. Background technique [0002] Nornicotine is one of the main alkaloids in smokeless tobacco products, which has an important impact on the quality of smokeless tobacco products, and is the precursor substance of tobacco-specific nitrosamine-nitrosonornicotine (NNN) . The nornicotine molecule contains a chiral center, so nornicotine has two enantiomers: S-(-)-nornicotine (referred to as S-nornicotine) and R-(+)-nornicotine (referred to as R-nornicotine). Depending on the identity of the enantiomers, the two enantiomers of nornicotine may have completely different metabolic mechanisms and physiological properties. Therefore, it is necessary to analyze and determine the enantiomer content of ...

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Problems solved by technology

[0003] At present, the methods for determining the enantiomers of nornicotine reported in the literature mainly include gas chromatography-mass spectrometry (GC-MS, Beiträge Zur Tabakforschung. 2013;25(7):649-659. Chirality. 1999;11(1 ):82-84.), multidimensional gas chromatography-mass spectrometry (MDGC-MS, J. Chromatogr. B. 2008;865(1):13-17.), capillary electrophoresis (CE, Electrophoresis. 2009;30 (2):349–356.), etc., however, GC-MS and MDGC-MS need to be derivatized in the pretreatment process, which is time-consuming and laborious. CE only uses retention time for qualitative, which has relatively poor qualitative ability and is prone to false positives. positive result

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