高效液相色谱-内标法测定卷烟烟气粒相物中的B(a)P

Determination of Benzo[a]pyrene in cigarette smoke condensate by HPLC using internal standard

研究了使用1,2-二(9—蒽基)乙烷作为内标,高效液相色谱—荧光检测器(HPLC-FD)法测定卷烟烟气粒相物中B(a)P的方法。在捕集了卷烟烟气的剑桥滤片上加入内标,经超声萃取后用SPE小柱进行纯化。萃取液浓缩重组溶剂后直接进样分析。优化了流动相并选择了梯度洗脱使得B(a)P与内标物完全分离。使用该方法测定商品卷烟,方法平均回收率为(94±1.2)%,方法检测限是0.9ng/mL,相对标准偏差为(3.1～3.8)%。

An accurate and effective method of utilizing high-performance liquid chromatography （HPLC） with fluorescence detection （FD） by taking 1,2-bis （9-anthryl）ethane as an internal standard （I. S. ） was developed for the determination of benzo[a]pyrene （BaP） in cigarette smoke condensate. The method involves an ultrasonic extraction of Cambridge filters with cyclohexane followed by a solid-phase extraction on a Si cartridge for cleanup. After being concentrated and solvent reconstituted, samples were directly injected. The optimized mobile phase, which contained a gradient prepared from acetonitrile-tetrahy- drofuran （THF）-water, 75 ： 10：15 （v/v） （mixture A） and acetonitrile-water, 70：30 （v/v） （mixture B）, allowed the com- plete separation of I.S. and BaP. This method was applied to analyze 7 cigarette samples from China. Method recovery achieved was （94± 1.2）% （Mean± SD, %） with a relative standard derivation （RSD, %） ranging from 3.1 to 3.8. The limit of the detection （LOD） was found to be 0.9 ng/mL.