液相色谱-串联质谱法测定小型家用电器塑料部件中全氟辛酸  

Determination of Perfluorooctanoic Acid(PFOA) in Plastic Component of the Household Appliances by High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：张岩[1,2] 庞坤 吕品[3] 李挥 卢晓宇[1] 

机构地区：[1]北京出入境检验检疫局,北京100026 [2]河北省食品质量监督检验研究院,河北石家庄050091 [3]河北医科大学,河北石家庄050017

出　　处：《分析测试学报》2012年第4期486-490,共5页Journal of Instrumental Analysis

基　　金：国家质检总局科技计划项目(2007IK270)

摘　　要：建立了高效液相色谱-串联质谱(HPLC-MS/MS)结合加速溶剂萃取测定小型家用电器塑料部件中全氟辛酸(PFOA)的分析方法。样品冷冻粉碎后采用甲醇作溶剂进行快速溶剂萃取,萃取液经C18固相萃取柱富集净化后,以C18柱为分离柱,以甲醇-水为流动相,梯度洗脱,电喷雾负离子模式下多反应监测(MRM))模式检测。PFOA在0.5～100.0μg/L范围内线性关系良好(r2=0.998 9),回收率为93%～107%,相对标准偏差为2.9%～7.6%,检出限(S/N=3)为0.5μg/kg。该方法操作简便、灵敏度高,适用于小型家用电器塑料部件中全氟辛酸残留分析。A method based on high performance liquid chromatography tandem mass spectrometry（HPLC-MS/MS） with accelerated solvent extraction（ASE） was developed for the quantitative detection of perfluorooctanoic acid（PFOA） in plastic component of the household appliances.The sample was extracted with accelerated solvent extraction using methanol as extraction solvent.The extract were purified and enriched on a C18 column by solid phase extraction（SPE） column.The target compound was separated on a C18 column using methanol-water as mobile phase by gradient elution,and detected by MS with electrospray ionization（ESI） under multiple reaction monitoring（MRM） mode.The calibration curve was linear in the range of 0.5-100.0 μg/L with a correlation coefficient（r2） of 0.998 9.The recoveries for PFOA were in the range of 93%-107% with relative standard deviations of 2.9%-7.6%.The detection limit（S/N=3） was 0.5 μg/kg.The method is easy-handling,time-saving and sensitive,and is suitable for the determination of PFOA in plastic component of household appliances.

关 键 词：高效液相色谱-串联质谱 全氟辛酸 家用电器塑料部件 加速溶剂萃取 

分 类 号：O657.63[理学—分析化学] TQ423[理学—化学]