同位素稀释三重串联四级杆质谱法测定鱼组织中24种多环芳烃  

Determination of 24 polycyclic aromatic hydrocarbons in fish tissue by isotope dilution GC-MS/MS

作　　者：曾浩[1] 汤桦[2] 陈大舟[2] 王冠男[1] 冯洁[1] 汪瑾彦[1] 李蕾[1] 

机构地区：[1]北京化工大学理学院,北京100029 [2]中国计量科学研究院化学计量与分析科学研究所,北京100013

出　　处：《分析试验室》2011年第9期11-16,共6页Chinese Journal of Analysis Laboratory

基　　金：科技部科技基础性工作专项课题(21-08-4GZ-5)资助

摘　　要：采用气相色谱-三重串联四级杆质谱联用技术测定了鱼组织中24种多环芳烃(PAHs)。将冻干鱼组织样品加入同位素内标后,用加速溶剂萃取法(ASE)进行提取,提取液采用凝胶排阻色谱(GPC)和固相萃取(SPE)联用进行净化。采用二氯甲烷为提取溶剂,100℃下提取,以二氯甲烷作为GPC的流动相,在3.5 mL/min流速下,收集9～23 min的流出液,用中性氧化铝SPE小柱净化,用7 mL V(环己烷)∶V(二氯甲烷)=3:7的溶液洗脱,洗脱液浓缩至200μL,采用气相色谱-三重串联四级杆质谱结合同位素稀释质谱法进行定性和定量检测。24种PAHs的平均回收率为86.8%～117.1%,RSD为0.21%～3.4%,检测限为0.05～0.90μg/kg。对5种鱼组织分析测定,样品中PAHs的质量分数为0.11～99.2μg/kg。A method for the determination and the quantification of 24 polycyclic aromatic hydrocarbons（PAHs） in freezing dried fish tissue was established by GC-MS/MS.24 PAHs were extracted with dichloromethane by accelerated solvent extraction（ASE）.Then the gel permeation chromatography（GPC） and solid phase extraction（SPE） were used for Purification.Dichloromethane was chosen as mobile phase and V（cyclohexane）∶V（dichloromethane） =3∶7 was chosen as eluting solution of SPE after optimizing the type and ratio of eluting solution.24PAHs were quantified by GC-MS/MS,using deuterated PAHs as internal standards,singlepoint method.the multiple reaction monitoring（MRM） condition of GC-MS/MS was optimized.The recoveries of 24 PAHs are between 86.8%and117.1% with relative standard deviations of 0.21%~3.32%（n=5）.The detection limits of 24PAHs are 0.05~0.90 μg/kg（dry weight）.The method was then applied to the determination of PAHs in five fish samples.24PAHs were found to be present at levels ranging from 0.11 to 99.22 μg /kg dry samples.This method will be successfully applied to the qualitative and quantitative analysis of fish tissue samples.

关 键 词：多环芳烃 同位素稀释质谱法 气相色谱-三重串联四级杆质谱 鱼组织 

分 类 号：O657.63[理学—分析化学]