凝胶净化-超高效液相色谱法测定卷烟主流烟气中的苯并[a]芘  

Study on the determination of benzo[a]pyrene in mainstream cigarette smoke by ultra-high performance liquid chromatography and sample preparation with gel permeation purification

作　　者：张霞[1] 刘志华[1] 孔维松[1] 刘巍[1] 崔柱文 胡秋芬[2] 陈永宽[1] 缪明明[1] 

机构地区：[1]云南省烟草化学重点实验室,云南烟草科学研究院,昆明650106 [2]云南民族大学化学与生物技术学院,昆明650031

出　　处：《分析试验室》2013年第10期99-102,共4页Chinese Journal of Analysis Laboratory

基　　金：云南中烟公司科技项目(2012JC02)资助

摘　　要：研究了用凝胶净化-超高效液相色谱测定卷烟主流烟气中的苯并[a]芘的方法,采用环己烷对捕集有卷烟主流烟气总粒相物的剑桥滤片进行超声萃取,萃取液经浓缩后用凝胶系统净化,以环己烷为流动相,Waters Styragel脂溶性凝胶柱为固定相分离,流速为2.0 mL/min,收集在16.8～20.4 min之间的流出液,然后用超高效液相色谱-荧光检测器测定,色谱柱为Waters ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7μm),流动相为乙腈-水,流速为0.6 mL/min。在选定条件下,苯并[a]芘的检出限为0.3 ng/cig,样品加标回收率为93.4%～96.3%,日内相对标准偏差为3.8%,日间相对标准偏差为4.1%;结果令人满意。A new method for the determination of benzo[a]pyrene in mainstream cigarette smoke by ultra-high performance liquid chromatography（UPLC） and sample preparation with gel permeation purification was studied.The total particulate matter of cigarette smoke was selected by the cambridge filter.Benzo[a]pyrene was extracted from the total particulate matter with ultrasonic extraction.The extract was purified by gel permeation purification.Benzo[a]pyrene was separated on a Waters ACQUITY UPLC BEH C 18（2.1 mm × 100 mm,1.7 μm） column with acetonitrile and water as mobile phase at a flow-rate of 0.6 mL /min.This method was applied to the determination of benzo[a]pyrene mainstream cigarette.Under the optimum conditions,the detection limit of benzo[a]pyrene was 0.3 ng / cig,the relative standard derivation of intra-day variation was 3.8%,and the relative standard derivation of inter-day variation was 4.1%.The recoveries ranged from 93.4% to 96.2%.

关 键 词：凝胶净化 超高效液相色谱 卷烟主流烟气 苯并[A]芘 

分 类 号：O657.7[理学—分析化学]