title: Rapid determination of six carcinogenic primary aromatic amines in mainstream cigarette smoke by two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry.
abstract: A fully automated, rapid, and reliable method for simultaneous determination of six carcinogenic primary aromatic amines (AAs), including o-toluidine (o-TOL), 2, 6-dimethylaniline (2, 6-DMA), o-anisidine (o-ASD), 1-naphthylamine (1-ANP), 2-naphthylamine (2-ANP), and 4-aminobiphenyl (4-ABP), in mainstream cigarette smoke was established. The proposed method was based on two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry (SPE/LC-MS/MS). The particulate phase of the mainstream cigarette smoke was collected on a Cambridge filter pad and pretreated via ultrasonic extraction with 2% formic acid (FA), while the gas phase was trapped by 2% FA without pretreatment for determination. The two-dimensional online SPE comprised of two cartridges with different absorption characteristics was applied for sample pretreatment. Analysis was performed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) under multiple reaction monitoring mode. Each sample required about 0.5h for solid phase extraction and analysis. The limit of detections (LODs) for six AAs ranged from 0.04 to 0.58ng/cig and recoveries were within 84.5%-122.9%. The relative standard deviations of intra- and inter-day tests for 3R4F reference cigarette were less than 6% and 7%, respectively, while no more than 7% and 8% separately for a type of Virginia cigarette. The proposed method enabled minimum sample pretreatment, full automation, and high throughput with high selectivity, sensitivity, and accuracy. As a part of the validation procedure, fifteen brands of cigarettes were tested by the designed method.
authors.affiliation: Quality Supervision & Test Center, China National Tobacco Corporation Shandong Branch, Jinan 250098, China.
authors.forename: Zhenying
authors.initials: Z
authors.lastname: Bie
authors.affiliation: Quality Supervision & Test Center, China National Tobacco Corporation Shandong Branch, Jinan 250098, China.
authors.forename: Wei
authors.initials: W
authors.lastname: Lu
authors.affiliation: Quality Supervision & Test Center, China National Tobacco Corporation Shandong Branch, Jinan 250098, China.
authors.forename: You
authors.initials: Y
authors.lastname: Zhu
authors.affiliation: Quality Supervision & Test Center, China National Tobacco Corporation Shandong Branch, Jinan 250098, China.
authors.forename: Yusong
authors.initials: Y
authors.lastname: Chen
authors.affiliation: Quality Supervision & Test Center, China National Tobacco Corporation Shandong Branch, Jinan 250098, China.
authors.forename: Hubo
authors.initials: H
authors.lastname: Ren
authors.affiliation: Quality Supervision & Test Center, China National Tobacco Corporation Shandong Branch, Jinan 250098, China. Electronic address: jls1280@163.com.
authors.forename: Lishun
authors.initials: L
authors.lastname: Ji
mesh_terms: D015057:1-Naphthylamine / Q000032:analysis; D000611:Aminobiphenyl Compounds / Q000032:analysis; D000814:Aniline Compounds / Q000032:analysis; D002273:Carcinogens / Q000032:analysis*; D002853:Chromatography, Liquid; D057230:Limit of Detection; D012906:Smoke / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D062789:Tobacco Products / Q000145:classification; D014052:Toluidines / Q000032:analysis
chemical_list: D000611:Aminobiphenyl Compounds; D000814:Aniline Compounds; D002273:Carcinogens; D012906:Smoke; D014052:Toluidines; C006757:4-biphenylamine; C007766:2,6-xylidine; D015057:1-Naphthylamine; C023622:2-toluidine; C003898:2-anisidine
keywords: Liquid chromatography tandem mass; Mainstream cigarette smoke; Online solid phase extraction; Primary aromatic amines; Two-dimensional