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Method of measuring content of nornicotine enantiomer in cigarette cut tobacco through bonded phase chromatography-tandem mass spectrometry

A technology of enantiomer and tandem mass spectrometry, which is applied in the field of determination of enantiomer content of nornicotine in shredded cigarettes by phase convergence chromatography-tandem mass spectrometry, can solve the problems of time-consuming and laborious, poor qualitative ability and prone to false positives Results and other issues, to achieve the effect of short analysis time, good resolution and best extraction efficiency

Inactive Publication Date: 2017-10-13
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

Method used

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  • Method of measuring content of nornicotine enantiomer in cigarette cut tobacco through bonded phase chromatography-tandem mass spectrometry
  • Method of measuring content of nornicotine enantiomer in cigarette cut tobacco through bonded phase chromatography-tandem mass spectrometry
  • Method of measuring content of nornicotine enantiomer in cigarette cut tobacco through bonded phase chromatography-tandem mass spectrometry

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Embodiment 1

[0032] 1. Instruments and reagents

[0033] ACQUITY UPC2 ultra-high performance convergence chromatograph (Waters, USA), 6410B triple quadrupole mass spectrometer (Agilent, USA), AE163 electronic balance (sensitivity: 0.0001 g, Mettler, Switzerland), high-speed pulverizer (Wuhan Yincai Technology Co., Ltd.), ColeparmerVotex-Genie vortex oscillator in the United States, and SIGMA 3-30K-high-speed desktop refrigerated centrifuge in Germany. Dichloromethane (chromatographically pure), sodium hydroxide (analytical pure), formic acid (chromatographically pure), methanol (chromatographically pure), S-nornicotine standard, R-nornicotine standard.

[0034] 2. Sample preparation

[0035] (1) Mixing of shredded cigarette tobacco samples: Place the shredded cigarette tobacco samples in an oven at 40 °C, take out the shredded cigarette tobacco after 1 hour, crush them and pass them through a standard sieve with an aperture of 0.45 mm.

[0036] (2) Extraction of shredded cigarette tobacc...

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Abstract

The invention discloses a method of measuring content of nornicotine enantiomer in cigarette cut tobacco through bonded phase chromatography-tandem mass spectrometry. The method is characterized in that a cigarette cut tobacco sample is dried, smashed and screened, after being soaked in sodium hydroxide solution, the sample is extracted with dichloromethane, after matrix solid-phase dispersion is carried out on extract liquid, two-chiral-column tandem-bonded phase chromatography-tandem mass spectrometry is used for analysis, and a peak area normalization method is used for quantitatively determining the ratio of S-nornicotine and R-nornicotine in the cigarette cut tobacco. According to the provided detection method, the sample extracting and purifying method is simple and efficient, contamination to chromatographic columns by the sample liquid can be reduced, and the bonded phase chromatography-tandem mass spectrometry is high in sensitivity and specificity, capable of eliminating false positive, short in analysis time and capable of meeting the requirement of chiral analysis of nornicotine in cigarette cut tobacco samples in batches.

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 shredded cigarette tobacco by phase convergence chromatography-tandem mass spectrometry. Background technique [0002] Nornicotine is one of the main alkaloids in cigarette shreds, which has an important impact on the quality of cigarettes, and is the precursor 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 nornicotine in shredded cigarette toba...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 韩书磊陈欢付亚宁刘彤侯宏卫胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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