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Method for measuring content of nornicotine enantiomers in electronic cigarette liquid with hybrid-phase chromatography-tandem MS (mass spectrometry)

A technology of e-cigarette liquid and enantiomers, which is applied in the field of physical and chemical analysis, can solve the problems that there is no determination of the enantiomer content of nornicotine, prone to false positive results, and poor qualitative ability, so as to avoid False positive results, good extraction efficiency, and good separation

Inactive Publication Date: 2017-12-22
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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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
In addition, the existing literature mainly focuses on the tobacco matrix, and there is no report on the method for determining the content of nornicotine enantiomers in e-cigarette liquid

Method used

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  • Method for measuring content of nornicotine enantiomers in electronic cigarette liquid with hybrid-phase chromatography-tandem MS (mass spectrometry)
  • Method for measuring content of nornicotine enantiomers in electronic cigarette liquid with hybrid-phase chromatography-tandem MS (mass spectrometry)
  • Method for measuring content of nornicotine enantiomers in electronic cigarette liquid with hybrid-phase chromatography-tandem MS (mass spectrometry)

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Embodiment 1

[0030] 1. Instruments and reagents

[0031] 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), ColeparmerVotex-Genie, USA Machine, German SIGMA 3-30K-high-speed desktop refrigerated centrifuge. Dichloromethane (chromatographically pure), sodium hydroxide (analytical pure), formic acid (chromatographically pure), methanol (chromatographically pure), S-nornicotine standard, R-nornicotine standard.

[0032] 2. Sample preparation

[0033] (1) Extraction of e-cigarette liquid samples: Weigh 0.3 g of the sample into a 15 mL stoppered centrifuge tube, add 2.0 mL of 5% sodium hydroxide solution, vortex for 1 min to mix, and then let stand for 10 min to infiltrate the sample. Take 10 mL of dichloromethane into a centrifuge tube and shake at 4000 rpm for 30 min on a vortex mixer.

[0034] (2) Purification of the extract: Take 1.5 ...

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Abstract

The invention discloses a method for measuring content of nornicotine enantiomers in an electronic cigarette liquid with hybrid-phase chromatography-tandem MS (mass spectrometry). The method is characterized by comprising steps as follows: after being wetted with a sodium hydroxide solution, an electronic cigarette liquid sample is extracted with dichloromethane, an extraction liquid after being subjected to matrix dispersive solid-phase extraction and purification is analyzed with two-chiral-column series-connection-hybrid phase chromatography-tandem MS, and a ratio of S-nornicotine to R-nornicotine in the electronic cigarette liquid is detected quantitatively with a peak area normalization method. According to the detection method, the sample extraction and purification method is simple and efficient, pollution of the sample liquid to a chromatographic column can be reduced, and the detection method based on the hybrid-phase chromatography-tandem MS is high in sensitivity, good in specificity and short in analysis time, can remove false positive and can meet the requirement of chiral analysis for nornicotine in mass electronic cigarette liquid samples.

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 electronic cigarette liquid by phase convergence chromatography-tandem mass spectrometry. Background technique [0002] Electronic cigarettes, also known as electronic nicotine delivery systems, can atomize the smoke liquid in the cartridge through the built-in atomizer and deliver the atomized gas to the mouth and lungs, and the atomized gas often contains different concentrations of nicotine nicotine. Due to cost considerations, the nicotine added to e-cigarette liquid is basically derived from tobacco extraction. In addition to nicotine, tobacco also contains other minor alkaloids. The alkaloids with more content in tobacco and more people's research mainly include nornicotine, anatabine, anatabine, mesmin, etc. These Minor alkaloids also have certain biological activities a...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
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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