固相萃取新装置净化-超高效液相色谱法测定卷烟主流烟气中的苯并[α]芘  

Study on the determination of benzo[α]pyrene in mainstream cigarette smoke by UPLC and sample preparation with solid phase extraction new device

作　　者：许永 李晶 王晋 刘欣 孔维松 杨叶昆 杨光宇 李雪梅 黄海涛 XU Yong;LI Jing;WANG Jin;LIU Xin;KONG Wei-song;YANG Ye-kun;YANG Guang-yu;LI Xue-mei;HUANG Hai-tao(Technology center China tobacco Yunnan industrial Co., Ltd, Kunming 650106)

机构地区：[1]云南中烟工业有限责任公司技术中心,昆明650106

出　　处：《分析试验室》2018年第6期706-710,共5页Chinese Journal of Analysis Laboratory

基　　金：中国烟草总公司标准预研项目(2016QB007)资助

摘　　要：研究了用正相固相萃取净化,超高效液相色谱测定卷烟主流烟气中苯并[α]芘的方法。捕集有卷烟主流烟气总粒相物的剑桥滤片置于自主设计的样品萃取瓶中,用环己烷-乙醇(95:5,V/V)超声振荡萃取,提取液用硅胶固相萃取净化,然后以Waters ACQUITY UPLC BEH C18(2.1×50 mm,1.7μm)色谱柱为固定相,甲醇为流动相,超高效液相色谱-荧光检测测定;苯并[α]芘检出限为0.22 ng/支,样品加标回收率为89.6%~95.4%,日内相对标准偏差为3.2%,日间相对标准偏差为3.6%;结果令人满意。A new method for the determination of benzo[α]pyrene in mainstream cigarette smoke by UPLC and sample preparation with solid phase extraction was studied.The total particulate matter of cigarette smoke was collected with cyclohexane-ethanol（95： 5,V/V） by the Cambridge filter.The benzo[α]pyrene was extracted from the total particulate matter with ultrasonic extraction.The extract was purified by solid phase extraction.The benzo[α]pyrene was separated on a Waters ACQUITY UPLC BEH C18（2.1 × 50 mm,1.7μm） column with methanol as mobile phase at a flowrate of 0.5 m L/min,and detected with fluorescence detector.This method was applied to the determination of benzo[α]pyrene mainstream cigarette.The detection limit of benzo[α]pyrene was 0.22 ng/cig,the relative standard derivation of intra-day variations was 3.2%,the relative standard derivation of interday variations was 3.6%,and the recoveries were ranged from 89.6%-95.4%.

关 键 词：苯并[α]芘 超高效液相色谱 固相萃取 卷烟主流烟气 

分 类 号：S132[农业科学—农业基础科学]