同位素稀释-气相色谱-三重四极杆串联质谱法分析食用油中18种多环芳烃  

Determination of 18 Polycyclic Aromatic Hydrocarbons in Edible Oils by Isotope Dilution GC-MS/MS

作　　者：许婷[1] 汤桦[2] 陈大舟[2] 李蕾[1] 

机构地区：[1]北京化工大学环境有害化学物质分析北京市重点实验室,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：《质谱学报》2015年第2期120-127,共8页Journal of Chinese Mass Spectrometry Society

基　　金：国家质检总局"双打"重点产品检验鉴定技术方法验证评价项目(2012104001)资助

摘　　要：建立了同位素稀释气相色谱-三重四极杆串联质谱测定食用油中18种多环芳烃的方法,同时对前处理过程中固相萃取柱的选择、净化条件及离子源温度等条件进行了优化。样品与环己烷以1∶1（V/V）混匀后,采用分子印迹固相萃取柱串联石墨化碳黑柱浓缩与净化,多反应监测扫描模式下进行质谱检测。结果表明：线性范围为1-200μg/kg时,该方法线性关系良好（R2〉0.999）,检出限为0.03-0.27μg/kg,定量限为0.10-0.89μg/kg;添加水平在5、10、50μg/kg时,前处理回收率为67.9%-100.8%,精密度（n=3）为0.5%-8.7%。应用该方法检测市场上常见的食用油,未发现食用油中多环芳烃含量超标的现象。该方法可靠性高、速度快、灵敏度高,可用于食用油中多环芳烃的准确检测和标准物质定值。A method ID GC （V/V） the determination of 18 PAHs MS/MS. The oil samples were mixed with cyc lion and the coupled quantifi cleaned up by molecularly imprinted in edible oils was developed by lohexane in the ratio of 1 ： 1 solid-phase extraction （SPE） to graphitized carbon blacks solid phase extraction cartridge. Identifica were performed using GC; MS/MS in MRM mode. In the method, and GC MS/MS conditions were optimized, such as the selection of SPE columns, clean-up conditions on the tandem columns, the temperature of the ionsource. The method shows satisfactory linearity （R^2〉0.999） over the range assayed （1-200 μg/kg）, and the LODs range from 0.03 to 0.27 μg/kg, and the LOQs range from 0. 10 to 0.89 μg/kg. The pre-tre-tment recoveries using this method at lhree is in the range of 0.5%-8.7%. The proposed analytical method has been successfully applied for the analysis of 18 PAHs in edible oils obtained from Beijing market. The results indicate that all the detected edible oil samples meet the requirement of China and EU regulation. This indicates that the developed method is suitable for the simultaneous determination and valued of 18 PAHs in edible oils.

关 键 词：同位素稀释质谱(ID-MS) 多环芳烃(PAHs) 食用油 分子印迹固相萃取柱(MISPE) 气相色谱-三重四极杆质谱(GC-MS/MS) 

分 类 号：O657.63[理学—分析化学]