Means J C, Hulebak K L
Neurotoxicology. 1983 Spring;4(1):37-43.
Exposure to methyltin compounds results in morphologically detectable damage to several mammalian organ systems. Although reliable dose-response relationships have been described, a fast method for quantitating levels of various methyltin species in target organs has been unavailable. It has been possible to measure organotins as total tin using atomic absorption spectrometry, but speciation of methyltins has proved difficult. We present a rapid method for quantitative analysis and speciation of methyltins, direct from mammalian tissues. Methyltin compounds (monomethyltin trichloride, dimethyltin dichloride, trimethyltin chloride, and tetramethyltin) are purged from freshly homogenized mouse kidney and brain tissues using NaBH4. The volatile organotin hydrides produced are cryogenically trapped on the head of a gas chromatographic column (at -40 degrees C) and eluted using a linear temperature program (15 degrees C/min to 190 degrees C). The compounds are detected using selected ion monitoring in a Hewlett Packard 5985-B mass spectrometer. Quantitation is achieved by integration of the areas of the chromatographic peaks. Linear response is obtained over the range of 1 ng to 30 micrograms for each compound. Recoveries of methyltins spiked into tissues are greater than 85%.
接触甲基锡化合物会导致多种哺乳动物器官系统出现形态学上可检测到的损伤。尽管已经描述了可靠的剂量-反应关系,但一直没有一种快速方法来定量目标器官中各种甲基锡物种的含量。使用原子吸收光谱法可以将有机锡作为总锡进行测量,但甲基锡的形态分析已证明很困难。我们提出了一种直接从哺乳动物组织中对甲基锡进行定量分析和形态分析的快速方法。使用NaBH₄从新鲜匀浆的小鼠肾脏和脑组织中吹扫出甲基锡化合物(三氯化一甲基锡、二氯化二甲基锡、氯化三甲基锡和四甲基锡)。产生的挥发性有机锡氢化物在气相色谱柱的柱头(-40℃)低温捕集,并使用线性升温程序(15℃/分钟至190℃)洗脱。在惠普5985-B质谱仪中使用选择离子监测来检测这些化合物。通过对色谱峰面积进行积分来实现定量。每种化合物在1 ng至30 μg范围内获得线性响应。添加到组织中的甲基锡回收率大于85%。