摘要
目的：以新型的加速溶剂萃取技术，结合稳定性同位素稀释气相色谱质谱法，建立测定食品巾20种指示性多氯联苯单体（PCBs）的方法。方法：样品中加入^13C12取代同位素后，经加速溶剂萃取、减压浓缩、混合硅胶柱与氧化铝柱净化后，洗脱液浓缩后用GC／MS测定，以选择离子监测方式监测目标化合物的特征离子，以内标法进行定量。以于贝和肉松为加标基质进行准确度和精密度试验，加标水平为0．5、1．0μg/kg。结果：以水产品和肉松为基质时，PCBs各单体的检测限分别为0．051—0．286、0．003—0．146μ/kg；除个别单体的回收率偏高（130％以上）外，其它单体的回收率均在86．4％-125．1％之间，相对标准偏差（RSD）在1．1％-19．6％之间，定量内标的回收率在68．8％-109．9％之间，满足痕量分析的要求。结论：本方法测定快速、定量准确可靠，可用于食品中20种指示性PCBs单体的测定。
Objective：To develop a method for determination of 20 indicator polychlorinated biphenyls（PCBs）in foodstuffs by GC-LRMS coupled with accelerated solvent extraction （ASE）. Methods： Samples were added with the stable isotope internal standard and was extracted by ASE. Extract parameters such as temperature, static cycles were optimized. The extract was analyzed by GC - MS - SIM after cleaned - up by multilayer silica column and alumina column. Results ： In the matrix of seafood and meat products, detection limits of 20 indicator PCBs were 0. 051 -0. 286,0. 003 -0. 146 μg/kg, respectively. Average recovery of PCBs was 86.4% - 125.1% when spiked at 0. 5 and 1.0 μg/kg in the dried scallop and pig fiber. And the relative standard deviation （RSD） varied from 1.1% to 19.6% （n = 5 ）. Recovery of the quantitative internal standard （IS） was 68.8% - 109.9%. Conclusion：The method is suitable for the rapid and accurate determination of 20 indicator PCBs in foodstuffs.
出处
《中国卫生检验杂志》
CAS
2006年第9期1025-1028,共4页
Chinese Journal of Health Laboratory Technology
基金
科技部"十五"科技攻关项目(2001BA804A19)
福建省卫生厅青年基金项目
关键词
多氯联苯
气相质谱分析
加速溶剂萃取法
稳定性同位素稀释
Polychlorinated biphenyls （PCBs）
Isotope dilution
GC -MS
Accelerated solvent extraction （ASE）
