提出了气相色谱法测定鲍鱼不同组织(肌肉、内脏、整贝)中的多氯联苯含量的方法。样品经正己烷超声萃取,硫酸净化后,肌肉样品只需再经过弗罗里硅土固相萃取小柱净化,内脏和整贝则还需经石墨化碳黑固相萃取小柱净化。用DB-5MS毛细管色谱柱分离,电子捕获检测器检测。7种多氯联苯的质量浓度在1.25~100 μg·L-1范围内与相应的峰面积呈线性关系,检出限(3S/N)在0.04~0.06 μg·kg-1之间。在0.25,2.50,20.0 μg·kg-1 3个浓度水平进行加标回收试验,回收率在78.0%~102%之间,测定值的相对标准偏差(n=5)在3.4%~6.9%之间。

A method of GC for the determination of polychloro-biphenyls in various tissues (muscle, viscera and whole cowry) of abalone was proposed. The samples were extracted ultrasonically with n-hexane and purified by sulfuric acid. Sample of muscle tissue was purified further by florisil solid phase extraction (SPE) column, while the samples of viscera tissue and whole cowry were purified further by both florisil SPE column and Carbon-GCB SPE column. The eluate was separated on DB-5MS capillary column and detected by ECD. Linear relationships between values of peak area and mass concentration of the 7 polychloro-biphenyls were kept in the same range of 1.25-100 μg·L-1 with detection limits (3S/N) in the range of 0.04-0.06 μg·kg-1. Tests for recovery were made at the concentration levels of 0.25, 2.50 and 20.0 μg·kg-1·L-1 of mixed standard, giving values of recovery and RSD′s (n=5) in the ranges of 78.0%-102% and 3.4%-6.9% respectively.