Watts R R, Hodgson D W, Crist H L, Moseman R F
J Assoc Off Anal Chem. 1980 Sep;63(5):1128-34.
A previously published method for determination and confirmation of hexachlorobenzene (HCB) in adipose tissue was also applied to mirex residues. A modified procedure for both residues was collaboratively studied by 12 laboratoires. The procedure specifies direct application of an extracted or rendered fat sample to a Florisil cleanup column and one-fraction elution. Mirex and HCB are determined by direct GLC of the concentrated eluate. HCB residues are then confirmed by reaction with isopropanol to form the disubstituted bis-isopropoxytetrachlorobenzene (BITB) derivative. Mirex residues are destroyed by this reaction. All participants were asked to analyze an unknown standard mixture of HCB and mirex and 10 rendered chicken fat samples consisting of one blank and 9 samples fortified samples represented 3 samples at each of 3 fortification levels. The HCB fortifications of 20.0, 33.3, and 50.0 ppb yielded average interlaboratory recoveries of 89.6, 87.4, and 92.6%, respectively. The respective coefficients of variation (CV) for HCB results were 9.1, 6,8, and 10.0%. The mirex fortifications of 150, 300, and 500 ppb yielded average interlaboratory recoveries of 89.0, 90.2, and 92.3%, respectively. The respective CV values for mirex results were 7.6, 16.5, and 18.1%. The method has been adopted official first action.
一种先前发表的用于测定和确证脂肪组织中六氯苯（HCB）的方法也被应用于灭蚁灵残留量的测定。12个实验室协同研究了针对这两种残留量的改进程序。该程序规定将提取或提炼后的脂肪样品直接应用于弗罗里硅土净化柱并进行单馏分洗脱。通过对浓缩洗脱液进行直接气相色谱法测定灭蚁灵和六氯苯。然后通过与异丙醇反应形成二取代双异丙氧基四氯苯（BITB）衍生物来确证六氯苯残留量。灭蚁灵残留量会因该反应而被破坏。要求所有参与者分析一份六氯苯和灭蚁灵的未知标准混合物以及10个提炼后的鸡脂肪样品，其中包括1个空白样品和9个加标样品，这些加标样品在3个加标水平下各有3个样品。六氯苯加标量为20.0、33.3和50.0 ppb时，实验室间平均回收率分别为89.6%、87.4%和92.6%。六氯苯结果的相应变异系数（CV）分别为9.1%、6.8%和10.0%。灭蚁灵加标量为150、300和500 ppb时，实验室间平均回收率分别为89.0%、90.2%和92.3%。灭蚁灵结果的相应CV值分别为7.6%、16.5%和18.1%。该方法已作为官方首次行动被采用。
