高分辨质谱法测定海鱼中二<inline-formula id="zgggws20041147-M1"><inline-graphic xmlns:xlink="http://www.w3.org/1999/xlink" href="zgggws20041147-M1.jpg"/></inline-formula>和多氯联苯

姜杰; 张建清; 蒋友胜; 周健; 张红宇

高分辨质谱法测定海鱼中二和多氯联苯

Determination on PCDD/Fs and Dioxin-like PCBs simultaneously in fish by isotope dilution HRGC/HRMS

摘要

摘要:
目的采用同位素稀释的HRGC/HRMS法定量检测鱼体中17种2, 3, 7, 8-氯取代的二(PCDD/Fs)和12种二多氯联苯(PCBs)。
方法参照美国EPA1613及EPA1668A方法, 采用索式抽提和自动纯化系统(FMS)对鱼体中的PCDD/Fs及PCBs进行纯化和富集、用同位素稀释气相色谱与高分辨质谱联用-多离子检测方法检测。
结果该方法可对样品中的PCDD/Fs及PCBs同系物进行有效分离, PCDD/Fs同位素标准物的回收率为83.83%~98.48%, PCBs同位素标准物的回收率为50.06%~90.56%。13种PCDD/Fs在鱼体中可检出, 总毒性当量(TEQ)为0.86pg/g, 12种二PCBs在鱼体中均可检测出, 总TEQ值为2.77pg/g。
结论该方法可以同时对同一样品中的17种PCDD/Fs及12种二PCBs进行检测, 检测效率高, 结果准确可靠。

Abstract:
Objective Seventeen PCDD/Fs and twelve dioxin-like PCBs in fish were determined by HR GC/HRMS.
Methods According to EPA1663 and EPA1668A, PCDD/Fs and PCBs were extracted from fish by Soxhlet extraction, cleaned up by FMS and quantified by HR GC/HRMS-M ID, using isotope dilution metholdogy.
Results The congeners of PCDD/Fs and PCBs can be separated well by this method. The recovery of PCDD/Fs was 83.83%-98.48%.The recovery of PCBs was 50.06%-90.56%.Thirteen congeners of PCDD/Fs and twelve congeners of PCBs can be detected in the fish. Total Toxicity Equivalency Quantity(TEQ)of PCDD/Fs in the fish was 0186 pg/g, TEQ of PCBs in the fish was 2177 pg/g.
Conclusion Seventeen congeners of PCDD/Fs and tweleve congeners of PCBs can be measured simultaneously in the same sample, the method was efficient and the results were accurate and reliable.

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