水和生物样品中痕量多氯联苯的分析方法研究

Studies on Analytical Method for Trace Polychlorinated Biphenyls Congeners in the Xenopus Laevis and Feeding Water

建立了一种水和生物体中痕量多氯联苯的提取、分离以及定性定量分析的新方法.本方法利用超声提取或液液萃取进行提取、硫酸硅胶柱和弗罗里土柱进行净化和分离,毛细管气相色谱进行分析,并优化了硫酸硅胶柱和弗罗里土柱净化分离多氯联苯的条件.水中痕量多氯联苯同类物的平均回收率为82%～115%;检出限为0.009～15.3 ng/L,生物样品中痕量多氯联苯同类物的平均回收率75%～135%;检出限为0.02～96.9 ng/g;相对标准偏差(RSD)均小于6.9%.方法用于实际水样和生物样品中痕量多氯联苯的分析,取得满意结果.

A novel method has been developed for the determination of trace polychlorinated biphenyls congeners in the biota samples and water. The method includes liquid-liquid extraction or ultrasonic extraction, cleanup of sulfuric acid silica column separation, separation of florisil column and analyses of capillary gas chromatography equipped with 63Ni electron-capture detection system （μ-ECD）. Conditions for cleanup of sulfuric acid silica gel column and separation of florisil column were optimized. The average recoveries were 82% - 115% for water, 75% - 135% for biotic samples, respectively. The limits of detection were 0. 009-15.3 ng/L for feeding water, from 0.02 to 96.9 ng/g for the biota samples, respectively, the relative standard deviations were all below 6.9%. The method was successfully used for the analyses of trace polychlorinated biphenyls congeners in Xenopus laevis and feeding water. The results of quality control show that the method merits the reliable investigation.