气相色谱-质谱联用同时测定蔬菜中16种邻苯二甲酸酯残留  

A simultaneous determination of 16 phthalates residues in vegetables by GC-MS/MS

作　　者：孙若男[1,3] 陈美瑜[2] 林竹光[3] 

机构地区：[1]山东出入境检验检疫技术中心,青岛266500 [2]厦门大学材料学院,福建省特种先进材料重点实验室,厦门361005 [3]厦门大学化学与化工学院,现代分析科学教育部重点实验室,厦门361005

出　　处：《分析试验室》2010年第12期73-76,共4页Chinese Journal of Analysis Laboratory

摘　　要：研究了蔬菜中16种邻苯二甲酸酯（PAEs）环境激素残留的气相色谱-电子轰击离子源质谱（GC-EI/MS）分析方法。优化了样品的前处理条件,以苯甲酸苄酯（BB）为内标物,采用GC-EI/MS的选择离子检测方式（SIM）进行定性和定量分析。当蔬菜样品的加标浓度水平分别为100和200μg/kg时,加标回收率为70.9%~123.0%,相对标准偏差为1.6%~15%。除邻苯二甲酸二甲氧基已酯（DMEP）外,其它15种PAEs的方法检测限（MDL）均为0.11~2.77μg/kg。在50.0~800.0μg/kg浓度范围内16种PAEs都呈现良好的线性关系,r为0.99623~0.99998。方法已用于5种蔬菜中16种痕量PAEs残留的分析。An analytical multiresidue method was developed for the simultaneous determination of 16 PAEs in vegetables by GC-EI/MS.Samples were extracted by hexane,cleaned up on a Florisil column,then were determined by GC-EI/MS with BB as the internal standard.The recovery studies were performed at 100 and 200 μg/kg fortification levels for each phthalate,and the recoveries ranged from 70.9% to 123.0% with a relative standard deviations between 1.6% and 15%.The detection limits of the method were less than 2.77 μg/kg for the most of PAEs except for DMEP.The developed method was linear over the range assayed 50~800 μg/kg,with determination coefficients in the range of 0.99623 ~0.99998.Finally,the developed analytical method was applied to the determination of 16 PAEs in five vegetables.

关 键 词：气相色谱-电子轰击离子源质谱 蔬菜 邻苯二甲酸酯 环境激素 

分 类 号：O657.63[理学—分析化学]