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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 method for the determination of benzo [a] pyrene in mainstream cigarette smoke by gel filtration and ultra-performance liquid chromatography was studied. The Cambridge filter which collected the total particulate matter in mainstream cigarette smoke was ultrasonographed using cyclohexane The extract was concentrated and purified by a gel system. Cyclohexane was used as the mobile phase. Waters Styragel lipophilic gel column was used as the stationary phase. The flow rate was 2.0 mL / min and the effluent was collected at 16.8-20.4 min Liquid and then determined by ultra performance liquid chromatography-fluorescence detector. The column was Waters ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, 1.7 μm). The mobile phase was acetonitrile-water and the flow rate was 0.6 mL / min. Under the selected conditions, the detection limit of benzo [a] pyrene was 0.3 ng / cig, the spiked recoveries were 93.4% -96.3%, the relative standard deviations were 3.8%, and the relative standard deviations were 4.1% The result is satisfactory.