Sasaki K, Ishizaka T, Suzuki T, Saito Y
National Institute of Hygienic Sciences, Division of Foods, Tokyo, Japan.
J Assoc Off Anal Chem. 1988 Mar-Apr;71(2):360-3.
An analytical method is described for the simultaneous quantitative determination of tri-n-butyltin and di-n-butyltin compounds in fish. The sample was extracted with 0.5N HCl-methanol, and the methanol solution was extracted with hexane. The extract was purified by gel permeation chromatography and treated with Grignard reagent to yield the methyl derivatives, which were determined by gas chromatography with flame photometric detection operated in the tin mode (610 nm). Recoveries of tri-n-butyltin chloride (Bu3SnCl) and di-n-butyltin dichloride (Bu2SnCl2) spiked to fish at the levels of 0.2 and 1.0 ppm ranged from 80 to 105%. Detection limits were 0.02 micrograms/g for both compounds. Tri-n-butyltin compounds equivalent to Bu3SnCl levels of 0.07-2.0 ppm and di-n-butyltin compounds equivalent to Bu2SnCl2 levels of 0.02-0.11 ppm were found in reared yellowtails, and these values showed good agreement with the results from gas chromatographic-mass spectrometric analysis.
本文描述了一种同时定量测定鱼类中三正丁基锡和二正丁基锡化合物的分析方法。样品用0.5N盐酸 - 甲醇萃取，甲醇溶液再用己烷萃取。萃取物通过凝胶渗透色谱法纯化，并用格氏试剂处理以生成甲基衍生物，通过气相色谱 - 火焰光度检测（锡模式，610nm）进行测定。向鱼中添加浓度为0.2和1.0ppm的三正丁基氯化锡（Bu3SnCl）和二正丁基二氯化锡（Bu2SnCl2）的回收率在80％至105％之间。两种化合物的检测限均为0.02微克/克。在养殖的黄尾鱼中发现相当于Bu3SnCl水平为0.07 - 2.0ppm的三正丁基锡化合物和相当于Bu2SnCl2水平为0.02 - 0.11ppm的二正丁基锡化合物，这些值与气相色谱 - 质谱分析结果吻合良好。
