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LC-MS/MS法检测卷烟滤嘴截留的烟气TSNAs

Analysis of Tobacco-Specific Nitrosamines in Cigarette Smoke Removed by Filter with LC-MS/MS

  • 摘要: 为了解滤嘴对烟草特有亚硝胺(TSNAs)的截留效率,采用液相色谱-串连质谱(LC-MS/MS)法测定了30种卷烟样品滤嘴中截留的烟气TSNAs:NNN、NAT、NNK、NAB。用0.1mol/L醋酸铵水溶液萃取烟蒂滤嘴,萃取液过OASIS MCX小柱,用50%(体积分数)甲醇洗脱,洗脱液直接进行LC-MS/MS分析,分析条件为:色谱柱:Waters Symmetry Shield TM RP18柱,柱温:65℃;流动相:50%甲醇水溶液(水中含0.1%醋酸),等度洗脱,流速0.25mL/min。结果显示:①NNN、NAT、NNK和NAB的检测限分别为0.7、0.3、0.6和0.4ng/支,回收率96.0%~103.5%,相对标准偏差(RSD)均小于8%;②NNN、NNK、NAT、NAB的滤嘴截留率分别在16.67%~43.05%、30.51%~55.97%、16.19%~45.00%和41.68%~49.08%范围内;③混合型卷烟滤嘴对NNN、NAT的截留效率要高于烤烟型卷烟,而对NNK、NAB和TSNAs总量,混合型卷烟滤嘴和烤烟型卷烟滤嘴的接近;④醋酸纤维滤嘴对NNK、NAB的截留率与聚丙烯纤维滤嘴相当,对NNN、NAT的截留率高于聚丙烯纤维滤嘴。

     

    Abstract: In order to investigate the removal efficiency of filter to tobacco-specific nitrosamines(TSNAs),the TSNAs in cigarette smoke,NNN,NAT,NNK and NAB,captured by the filters of 30 cigarette samples were determined by liquid chromatography and tandem mass spectrometry(LC-MS/MS).The filters were cut off the butts after smoking and extracted with 0.1 mol/L ammonium acetate aqueous solution.The resultant extraction passed through an OASIS MCX column,eluted with 50%(v/v) methanol,and analyzed by LC-MS/MS directly.The analytical conditions were:chromatographic column,Waters Symmetry Shield TM RP18,column temperature 65℃,mobile phase,50% of methanol-water(containing 0.1% acetic acid) solution at the flow rate of 0.25 mL/min and isogradient elution mode.The results showed that:1) the recoveries of NNN,NAT,NNK and NAB were from 96.0% to 103.5% with the relative standard deviations(RSD) of less than 8% and the limits of detection of 0.7,0.3,0.6 and 0.4 ng/cig.,respectively;2) the removal efficiencies of filters to NNN,NNK,NAT and NAB were 16.67% to 43.05%,30.51% to 55.97%,16.19% to 45.00%,and 41.68% to 49.08%,respectively;3) the NNN and NAT removal efficiencies of the filters attached to blended type cigarettes were higher than those of the filters attached to Virginia type cigarettes,while the NNK,NAB and total TSNAs removal efficiencies of the filters of the two cigarette types were similar;4) the NNN and NAT removal efficiencies of cellulose acetate filter were higher than those of polypropylene filter,while NNK and NAB removal efficiencies of the two filters were similar.

     

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