Schenck F J, Calderon L, Podhorniak L V
U.S. Food and Drug Administration, Baltimore District Laboratory, MD 21201, USA.
J AOAC Int. 1996 Sep-Oct;79(5):1209-14.
A rapid, multiresidue solid-phase extraction (SPE) technique for determination of organochlorine pesticide and polychlorinated biphenyl (PCB) residues in nonfatty fish was modified for use with fatty fish. In the modified procedures, samples are extracted with acetonitrile, and the extract is cleaned up with both C18 and Florisil SPE columns. Residues are determined by gas chromatography with electron capture detection. The original method was modified for use with fatty fish by reducing the amount of tissue extracted and by using an improved Florisil SPE cleanup. Recovery data are presented for 24 fortified organochlorine pesticide residues (0.12 ppm) and 3 fortified PCB residues (0.80 ppm) from flounder, bluefish, and shad samples, which contained 0.8, 5.4, and 22.6% fat, respectively. For the 3 types of fish, recoveries of 23 of 24 fortified organochlorine pesticide residues ranged from 55 to 129%, and recoveries of 3 fortified PCB residues ranged from 55 to 104%. There were no significant differences in recovery based on fish species and/or fat content for the majority of residues studied. This SPE method and the official AOAC method yielded comparable results for fish containing incurred organochlorine residues.
一种用于测定非脂肪鱼类中有机氯农药和多氯联苯（PCB）残留的快速多残留固相萃取（SPE）技术经过改进后可用于脂肪鱼类。在改进后的方法中，样品用乙腈萃取，萃取液通过C18和弗罗里硅土SPE柱进行净化。残留物通过带电子捕获检测的气相色谱法测定。通过减少萃取的组织量并使用改进的弗罗里硅土SPE净化方法，对原方法进行了改进以用于脂肪鱼类。给出了从分别含有0.8%、5.4%和22.6%脂肪的比目鱼、竹荚鱼和鲱鱼样品中加标24种有机氯农药残留（0.12 ppm）和3种加标PCB残留（0.80 ppm）的回收率数据。对于这3种鱼类，24种加标有机氯农药残留中的23种回收率在55%至129%之间，3种加标PCB残留的回收率在55%至104%之间。对于所研究的大多数残留，基于鱼类种类和/或脂肪含量的回收率没有显著差异。对于含有实际有机氯残留的鱼类，这种SPE方法与官方AOAC方法得出了可比的结果。
