气相色谱-串联质谱法测定虾体中18种多氯联苯

发布时间：2018-11-20 21:18

【摘要】：建立了基于气相色谱-串联质谱法测定虾体不同组织(虾肉、虾头、虾壳、虾黄)中7种环境指示类和12种类二VA英类多氯联苯(PCBs)的定性定量分析方法。样品经V(二氯甲烷):V(正己烷)=1:1混合溶液匀浆提取,加入浓硫酸磺化,采用弗罗里硅土柱净化。气相色谱部分采用HP-5柱,经程序升温对18种PCBs分离,进入串联四极杆质谱后,以EI~+离子源多反应监测模式(MRM)进行定性定量分析。结果表明:在50、400和1 000 ng/kg 3个添加水平下,18种PCBs在虾肉、虾头、虾壳和虾黄4种样品中的平均回收率在72%~109%之间,相对标准偏差均小于10%,18种PCBs的检出限在0.10~10 ng/kg之间。本方法具有较好精密度和准确度,前处理方法简单快速,可用于虾体中18种PCBs测定。对南京某养殖场的实际样品进行检测,只有部分PCBs检出。
[Abstract]:Based on gas chromatography-tandem mass spectrometry (GC-MS), a qualitative and quantitative analysis method was developed for the determination of 7 environmental indicator species and 12 species of dichlorobenzene polychlorinated biphenyls (PCBs) in different tissues (shrimp meat, shrimp head, shrimp shell, shrimp yellow). The sample was extracted by V (dichloromethane): V (n-hexane) = 1:1 mixed solution homogenate and sulphonated with concentrated sulfuric acid. In the gas chromatography, 18 kinds of PCBs were separated by programmed temperature on HP-5 column and entered into tandem quadrupole mass spectrometry. The qualitative and quantitative analysis was carried out by EI~ ion source multi-reaction monitoring mode (MRM). The results showed that the average recoveries of 18 kinds of PCBs in shrimp meat, shrimp head, shell and yellow shrimp were between 72% and 109%, and the relative standard deviations were less than 10% under the three additive levels of 50400 and 1 000 ng/kg. The detection limit of 18 PCBs was between 0.10 and 10 ng/kg. The method has good precision and accuracy, and the pretreatment method is simple and rapid. It can be used for the determination of 18 kinds of PCBs in shrimp body. Only a part of PCBs was detected from the actual samples of a farm in Nanjing.
【作者单位】：江苏省农业科学院食品质量安全与检测研究所;南京农业大学植物保护学院;
【基金】：江苏省农业科技自主创新项目[CX(15)1012-5]
【分类号】：TS254.7;O657.63

【相似文献】