Gas Chromatography-Tandem Mass Spectrometry Method for Selective Detection of 2-Nitropropane in Mainstream Cigarette Smoke.

Gala M Chapman, Juliana Giraldo Junco, Roberto Bravo Cardenas, Clifford H Watson, Liza Valentín-Blasini
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Abstract

Although 2-nitropropane is a potentially harmful compound present in cigarette smoke, there are few fully-validated, modern methods to quantitate it in mainstream cigarette smoke. We developed an isotope dilution gas chromatography-tandem mass spectrometry (ID-GC-MS/MS) method for the detection of 2-nitropropane in mainstream cigarette smoke. The vapor fraction of mainstream cigarette smoke was collected in inert polyvinyl fluoride gas sampling bags and extracted with hexanes containing isotopically labeled internal standard, then purified and concentrated via solid-phase extraction using a normal phase silica adsorbent and a 100% dichloromethane eluant. This method is sensitive enough to measure vapor phase 2-nitropropane concentrations in the nanogram range, with a 19 ng per cigarette method limit of detection. Product variability estimated from the analysis of 15 cigarette products yielded relative standard deviations ranging from 5.4% to 15.7%, and estimates of precision from two quality control products yielded relative standard deviations of 9.49% and 14.9%. Under the Health Canada Intense smoking regimen, 2-nitropropane in machine-generated mainstream smoke from 15 cigarette products ranged from 98.3 to 363 ng per cigarette.

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气相色谱-串联质谱法选择性检测主流卷烟烟雾中的2-硝基丙烷。
虽然2-硝基丙烷是香烟烟雾中存在的一种潜在有害化合物,但很少有经过充分验证的现代方法来量化主流香烟烟雾中的2-硝基丙烷。建立了一种同位素稀释气相色谱-串联质谱(ID-GC-MS/MS)检测主流卷烟烟雾中2-硝基丙烷的方法。采用惰性聚氯乙烯氟气体取样袋收集主流卷烟烟气蒸汽馏分,用含有同位素标记内标的己烷进行萃取,用正相二氧化硅吸附剂和100%二氯甲烷洗脱液进行固相萃取提纯浓缩。该方法具有足够的灵敏度,可以在纳克范围内测量气相2-硝基丙烷的浓度,每支香烟的检测限为19 ng。从对15种卷烟产品的分析中估计出的产品变异性产生了5.4%至15.7%的相对标准偏差,从两个质量控制产品估计的精度产生了9.49%和14.9%的相对标准偏差。根据加拿大卫生部的强烈吸烟方案,15种卷烟产品中机器产生的主流烟雾中的2-硝基丙烷含量为每支香烟98.3至363纳克。
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Beitrage zur Tabakforschung International/ Contributions to Tobacco Research
Beitrage zur Tabakforschung International/ Contributions to Tobacco Research Agricultural and Biological Sciences-Agronomy and Crop Science
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Gas Chromatography-Tandem Mass Spectrometry Method for Selective Detection of 2-Nitropropane in Mainstream Cigarette Smoke. LC-MS/MS Analysis of Sugars, Alditols, and Humectants in Smokeless Tobacco Products. Within-Laboratory Variance Outlier Detection: An Alternative to Cochran’s Test Estimation of the Retention of Menthol in the Respiratory Tract of Menthol Cigarette Smokers: A Pilot Study The Full Bibliography of Alan Rodgman
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