液相色谱-大气压光电电离源质谱法同时测定电子电气产品中16种多环芳烃残留  

Simultaneous Quantitative Determination of 16 Polycyclic Aromatic Hydrocarbons (PAHs) by HPLC-APPI-MS/MS

作　　者：殷居易[1] 谢东华[1] 陈建国[1] 章再婷[1] 俞雪钧[1] 刘罡一 陈允华 陈杰[1] 

机构地区：[1]宁波出入境检验检疫局技术中心食品安全分中心,浙江宁波315012 [2]上海徐汇区中心医院实验室,上海200031 [3]爱谱拜瑞斯美国应用生物系统公司,上海200040

出　　处：《质谱学报》2009年第5期300-306,310,共8页Journal of Chinese Mass Spectrometry Society

基　　金：国家标准化管理委员会(20090086-T-469)科技资助项目

摘　　要：采用HPLC-APPI-MS/MS法同时测定电子电器产品中橡胶,塑料等材料中的16种多环芳烃(PAHs)残留量。样品经粉碎后,用甲醇提取,通过C18小柱过柱净化,以液相色谱分离,大气压光电电离源离子化电离串联质谱进行检测,采用多反应监测模式同时测定16种多环芳烃浓度。该方法定量下限(LOQ,S/N>10)为0.1～0.2μg·g-1,回收率为72.0%～89.6%,变异系数小于10%。在0.1～10.0μg·L-1浓度范围内,峰面积与浓度呈良好线性(r:0.9932～0.9992)。An HPLC APPI（＋）MS MS method was developed by solid phase extraction decontamination for the residue determination of PAHs. The sample was extracted by the methyl alcohol after comminution and operating for decontamination by C18 cartridges. Samples were detected by a gradient elution flowing with a APPI positive mode detector at MRM（naphthalene m/z 128, acenaphthylene m/z 152, acenaphthene m/z 154, fluorene rn/z 166, phenanthrene m/z 178, anthracene m/z 178, fluoranthene m/z 202, pyrene m/z 202, benz（a）anthracene rn/z 228, chrysene rn/z 228, benzo（b）fluoranthene m/z 252, benzo（k）fluoranthene m/z 252, benzo（a）pyrene m/z 252, benzo（g,h,I）perylene m/z 276, indeno（1,2,3,c,d）pyrene m/z 276, dibenz（a,h）anthraeene m/z 278）. The LOQs （S/N〉 10）of 16 PAHs residues in the negative meat sample are 0.1-0.2 mg.kg^-1. The recovery values is 72.0%-89.6%. The response for 16 PAHS is linear in the range of 0.1-10.0μg.L^-1 , and the correlation coefficient is excellent（r. 0. 993 2-0. 999 2）.

关 键 词：液相色谱-大气压光电电离源质谱 电子电气产品 多环芳烃 

分 类 号：O657.63[理学—分析化学] S767.3[理学—化学]