LC-MS-MS法测定卷烟侧流烟气中的亚硝胺

采用鱼尾罩和剑桥滤片捕集卷烟侧流烟气中的粒相颗粒物,建立了LC-MS-MS法测定卷烟侧流烟气中4种烟草特有的亚硝胺TSNAs(NNN,NAT,NAB,NNK)。剑桥滤片在醋酸铵水溶液中机械振荡40min后提取萃取液,萃取液经0.22μm滤膜过滤后,直接进LC-MS-MS分析。鱼尾罩壁上的冷凝物用甲醇溶液清洗,洗液通过氮吹浓缩后,采用PCX固相萃取小柱净化进样分析。测定方法的检测限为0.09～0.25ng/mL,线性相关系数均大于0.996,4种TSNAs的回收率均在88.2%～110.2%之间,相对标准偏差RSD均小于7%。方法适合作为卷烟侧流烟气中四种烟草特有亚硝胺(TSNAs)的定量分析方法。

Determination of tobacco-specific nitrosamines in cigarette side stream smoke by LC-MS-MS

An analytical method for the determination of 4 kinds of tobacco specific nitrosamines(TSNAs) in cigarette side stream smoke was developed by LC-MS-MS.A fishtail chimney and Cambridge filter were used to capture the particulate matters consisting of TSNAs in side stream smoke.The Cambridge filter was put in a 250 mL conical flask with 100μL of internal standards solution and 20 mL of(100mmol/L)ammonium acetate solution and then shaken in mechanical oscillator for 40 minutes.The extract liquor was filtered through 0.22 μm filter membrane and analyzed by LC-MS-MS.The fishtail chimney eluent was concentrated and purified with PCX solid extraction,then analyzed by LC-MS-MS.Results: The limits of detection were in the range of 0.09~0.25ng/mL and linear correlation coefficients were above 0.996.The recoveries of 4 kinds of TSNAs ranged from 88.4% to 109.5% and the relative standard deviations were all below 7%;with high accuracy and sensitivity,the method can be used to determine TSNAs in cigarette sidestream smoke.