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Liquid chromatogram tandem mass spectrum measurement method for tobacco-specific nitrosamines in electronic cigarette liquid

A technology for e-cigarette liquid and determination method, which is applied to measurement devices, instruments, scientific instruments, etc., can solve problems such as unfavorable conventional analysis of TSNAs, cumbersome and other problems, and achieve the effects of simple pretreatment, good repeatability, and improved analysis throughput.

Inactive Publication Date: 2014-06-04
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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Problems solved by technology

Korean scholars have established liquid-liquid extraction, solid-phase extraction-LC-MS / MS methods for the determination of TSNAs in e-cigarette liquid, but the pretreatment of the method is cumbersome, including liquid-liquid extraction and solid-phase extraction, which is not conducive to e-cigarette liquid Routine analysis of TSNAs in

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  • Liquid chromatogram tandem mass spectrum measurement method for tobacco-specific nitrosamines in electronic cigarette liquid

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example 1

[0029] Example 1: 1. Instruments and reagents: Agilent 1200 liquid chromatography (Agilent, USA) with G1329A autosampler, G1311A quaternary mixing pump and G1316A, column oven; API 4000 triple quadrupole tandem mass spectrometer (Applied Biosystems, USA) ), equipped with an electrospray ionization source (ESI) and an analyst 1.5 software data processing system. NNK, NNN, NAT and NAB standards and NNK-d 4 , NNN-d 4 , NAT-d 4 and NAB-d 4 Purchased from Toronto Research Chemicals Inc., Canada, the purity is more than 98%; methanol, acetic acid and ammonium acetate are all chromatographic pure, and the water used in the experiment is deionized water.

[0030] 2. Sample processing: Accurately weigh 1.00 g of e-cigarette liquid sample and put it into a 10 mL volumetric flask; add 50 μL of 5 μg / mL tobacco-specific nitrosamines (NNK, NNN, NAT and NAB) mixed internal standard solution, Dilute to the mark with 100 mM ammonium acetate solution, and after sonicating for 10 min to mi...

example 2

[0032] Example 2: According to the assay method described in Example 1, 6 electronic cigarette smoke liquid samples were selected, and the content of tobacco-specific nitrosamines was measured as shown in Table 3.

[0033] Table 3 Content levels of tobacco-specific nitrosamines in samples (ng / g)

[0034] serial number NNK NNN NAT NAB 1 1.57 3.05 24.1 2.43 2 3.24 4.02 26.9 2.27 3 4.49 9.05 16.8 1.22 4 0.10 0.53 0 0 5 0.12 1.69 0 0 6 0 10.7 0 0

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Abstract

The invention discloses a liquid chromatogram tandem mass spectrum measurement method for tobacco-specific nitrosamines in electronic cigarette liquid. The liquid chromatogram tandem mass spectrum measurement method is characterized by comprising the step of directly introducing a liquid chromatogram-electrospray ionization-tandem mass spectrometer for measurement after the electronic cigarette liquid is diluted so as to quantify an analyte by adopting an internal standard method. The content of the tobacco-specific nitrosamines in the electronic cigarette liquid can be rapidly and accurately detected. According to the liquid chromatogram tandem mass spectrum measurement method for tobacco-specific nitrosamines in the electronic cigarette liquid, the selectivity and the accuracy of the method are well improved by using a tandem mass spectrography, quantification limits of NNK (Nicotine-derived Nitrosamine Ketone), NNN (N'-Nitrosonornicotine), NAT (N-Nitrosoanatabine) and NAB (N-Nitrosoanabasine) are respectively 0.08ng / mL, 0.10ng / mL, 0.12ng / mL and 0.09ng / mL, the recovery rate range of the method is 90.9-108.1 percent, and the RSD (Relative Standard Deviation) is less than 12.1 percent. By selecting and optimizing a chromatographic column and an elution condition, the chromatographic separation process is well improved, and the chromatographic analysis time is shortened to be 6min.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical testing of electronic cigarettes, in particular to a method for determining the content of tobacco-specific nitrosamines in electronic cigarette smoke liquid by using liquid chromatography-electrospray ionization-tandem mass spectrometer. Background technique [0002] 4-(Nitrosomethylamino)-1-β-pyridyl)-1-butanone (NNK), N -Nitrosonornicotine (NNN), N - Nitrosoanatabine (NAT) and N -Nitrosoanabasine (NAB) is a carcinogen widely present in cigarette smoke, and these substances only exist in tobacco products or cigarette smoke, so they are called tobacco-specific nitrosamines (TSNAs). The International Agency for Research on Cancer (IARC), the Hecht research team, etc., the results of the toxicity evaluation of the harmful ingredients in the Canadian government list show that there is sufficient evidence to believe that NNK in TSNAs is carcinogenic to laboratory animals. Therefore, ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 张小涛韩书磊陈欢刘彤吴帅宾侯宏卫胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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