Yurawecz M P, Roach J A
J Assoc Off Anal Chem. 1978 Jan;61(1):26-31.
1,2,3,4,7,7-Hexachloro-2,5-norbornadiene (I), 1,2,3,4,5-endo,7,7-heptachloro-2-norbornene (II), and 1,2,3,4,7,7-hexachloro-5,6-endo-epoxy-2-norbornene (III) have been identified as contaminants in Mississippi River fish by combined gas-liquid chromatography (GLC)-mass spectrometry. The method used to determine residues of these compounds, which are associated with production of the pesticide endrin, is similar to the AOAC multiresidue method for chlorinated pesticides. The residues are extracted from the sample with acetonitrile, transferred to petroleum ether, and chromatographed on a Florisil column. Compounds I and II are eluted from the Florisil with petroleum ether and compound III is eluted with ethyl ether-petroleum ether (6 + 94). The concentrated eluates are analyzed by using electron capture GLC. The method provides adequate recoveries of all 3 chlorinated norbornene derivatives and allows quantitation at or below the 0.05 ppm level in fish with a 20 mg sample equivalent injection.
通过气相色谱 - 质谱联用（GLC）法，已鉴定出1,2,3,4,7,7 - 六氯 - 2,5 - 降冰片二烯（I）、1,2,3,4,5 - 内型，7,7 - 七氯 - 2 - 降冰片烯（II）和1,2,3,4,7,7 - 六氯 - 5,6 - 内型 - 环氧 - 2 - 降冰片烯（III）为密西西比河鱼类中的污染物。用于测定这些与杀虫剂异狄氏剂生产相关的化合物残留量的方法，类似于美国官方分析化学师协会（AOAC）的氯化农药多残留方法。残留物用乙腈从样品中提取，转移至石油醚中，并在弗罗里硅土柱上进行色谱分析。化合物I和II用石油醚从弗罗里硅土中洗脱，化合物III用乙醚 - 石油醚（6 + 94）洗脱。浓缩后的洗脱液用电子捕获气相色谱法进行分析。该方法对所有3种氯化降冰片烯衍生物都有足够的回收率，并且在进样量相当于20mg鱼样时，能够对鱼类中0.05ppm及以下的含量进行定量分析。
