CAJ | 학술논문

建立了同时测定卷烟主流烟气中苯并[a]芘(BaP)和4-(N-甲基-N-亚硝氨基)-1-(3-吡啶基)-1-丁酮(NNK)的气相色谱-串联质谱(GC-MS/MS)方法.用剑桥滤片捕集卷烟主流烟气粒相物后再用甲苯进行振荡萃取,萃取液经过基质分散固相萃取净化及氮吹浓缩后采用DB-35MS色谱柱分离、多反应监测(MRM)模式分析,内标法定量.结果表明:①NNK和BaP的定量限、加标回收率、相对标准偏差(RSD)分别为0.36和0.29 ng/支,78.8%~95.5%和101.6%~106.6%,2.3%~15.4%和2.9%~14.4%.②与标准方法相比,该方法前处理简单,可实现两种目标物的同时测定.③采用该方法与现有标准方法对27个卷烟的检测结果显示两组数据的一致性较好,无显著性差异.该方法操作简单、结果准确,适用于同时分析卷烟主流烟气中NNK和BaP的释放量.
건립료동시측정권연주류연기중분병[a]비(BaP)화4-(N-갑기-N-아초안기)-1-(3-필정기)-1-정동(NNK)적기상색보-천련질보(GC-MS/MS)방법.용검교려편포집권연주류연기립상물후재용갑분진행진탕췌취,췌취액경과기질분산고상췌취정화급담취농축후채용DB-35MS색보주분리、다반응감측(MRM)모식분석,내표법정량.결과표명:①NNK화BaP적정량한、가표회수솔、상대표준편차(RSD)분별위0.36화0.29 ng/지,78.8%~95.5%화101.6%~106.6%,2.3%~15.4%화2.9%~14.4%.②여표준방법상비,해방법전처리간단,가실현량충목표물적동시측정.③채용해방법여현유표준방법대27개권연적검측결과현시량조수거적일치성교호,무현저성차이.해방법조작간단、결과준학,괄용우동시분석권연주류연기중NNK화BaP적석방량.
A method for simultaneously determining the benzo[a]pyrene (BaP) and 4-(N-methyl-N-nitrosamino)-1-(3-pyridyl)-1-butanone (NNK) in mainstream cigarette smoke by gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed. The total particulate matter of mainstream cigarette smoke was collected on a Cambridge filter pad, then extracted with toluene by oscillation. The extract was cleaned up by dispersive solid phase extraction (d-SPE), concentrated by nitrogen gas flow, separated by DB-35MS column, and determined by internal standard method under multi-reaction monitoring (MRM) mode. The results showed that: 1) The limits of quantitations (LOQs), recoveries and relative standard deviations (RSDs) of NNK and BaP were 0.36 and 0.29 ng/cig, 78.8%-95.5% and 101.6%-106.6%, 2.3%-15.4% and 2.9%-14.4%, respectively. 2) Comparing with the standard method, the developed method was simpler in pretreatment, and capable of simultaneous determination of the two target analytes. 3) The data of 27 cigarette samples determined by the developed method well agreed with those by the standard method, there was no significant difference. The method is simple, accurate and suitable for the simultaneous determination of NNK and BaP in mainstream cigarette smoke.