GC-MS/MS (Gas chromatography - tandem mass spectrometry) method for simultaneously analyzing three polycyclic aromatic hydrocarbons and four tobacco-specific nitrosamines in main stream smoke of cigarettes

Abstract

The invention discloses a GC-MS / MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing three polycyclic aromatic hydrocarbons and four tobacco-specific nitrosamines in main stream smoke of cigarettes. The method comprises the following steps of: taking out a Cambridge filter disc catching granule phase objects of main stream smoke of cigarettes, adding ethyl acetate and an internal standard, carrying out vibrating extraction, carrying out dispersive solid-phase extraction (d-SPE) on extracting liquid, then, carrying out nitrogen-blowing concentration on supernatant, and measuring by using GC-MS / MS. The method provided by the invention overcomes the problems that a sample treatment method can separately detect the two substances in the prior art and the pretreatment is tedious; and a sample pretreatment method and an instrument detection condition are optimized aiming at the granule phase objects of main stream smoke of cigarettes. The method provided by the invention has the advantages that two target objects with large polar phase differences are extracted at the same time by 10mL of ethyl acetate, and the extraction efficiency is high; and compared with the national standard method, the method has the advantages that the consumption of an organic solvent is reduced by a several times to tens of times, and the method has the characteristics of accurate operation, high sensitivity and good repeatability.

Description

technical field [0001] The invention belongs to the technical field of detection of harmful substances in cigarette smoke, and mainly relates to three polycyclic compounds such as benzo[a]anthracene (BaA), Chrysene and benzo[a]pyrene (BaP) in cigarette mainstream smoke. Determination techniques for aromatics and four tobacco-specific nitrosamines (TSNAs) including NNN, NAT, NAB, and NNK. [0002] Background technique [0003] Polycyclic aromatic hydrocarbons represented by benzo[a]pyrene and tobacco-specific nitrosamines (TSNAs) represented by NNK are two main types of harmful substances in mainstream cigarette smoke, which have strong carcinogenic effects and are harmful to animals or humans in the past. The weight analysis of toxicology studies shows that the strongest carcinogenic effects in tobacco are TSNAs and PAHs, which have always been the hotspots of people's research. [0004] Benzo[a]pyrene and tobacco-specific N-nitrosamines in cigarette mainstream smoke are o...

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Problems solved by technology

[0005] GC / MS method to measure polycyclic aromatic hydrocarbons in cigarette mainstream smoke generally uses organic solvents such as n-hexane or cyclohexane containing internal standard to extract the total particle phase of smoke The extract was purified with a silica gel solid-phase extraction column. After the eluate was concentrated, it was analyzed by GC / MS and quantified by the selected ion monitoring (SIM) mode, which has high recovery rate, high sensitivity, good repeatability, and accurate quantification, etc. characteristics, but the cumbersome solid-phase extraction process and concentration process are required in the sample pretreatment process, which is time-consuming and laborious, and it was found in the GC / MS detection process of polycyclic aromatic hydrocarbons in the mainstream smoke of cigarettes with tar content less than 1 mg / cig that benzene The content of benzo[a]pyrene is mostly lower than 1 ng / cig. At this time, the GC / MS chromatographic peak of benzo[a]pyrene is low, which brings certain difficulties to the quantification

[0006] For the determination of tobacco-specific N-nitrosamines in the total particulate matter of mainstream smoke by GC-TEA method, since the thermal energy analyzer only detects nitrosamines and nitrites The response is a specific detector, so it has quite high selectivity and sensitivity, but the disadvantage of this method is that there are many purification steps, long analysis time, and for flue-cured tobacco with extremely low N-nitrosamine content in tobacco , the sensitivity of GC-TEA is slightly insufficient

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