Arakawa Y, Wada O, Yu T H, Iwai H
J Chromatogr. 1981 Oct 30;216:209-17. doi: 10.1016/s0021-9673(00)82349-3.
Taking advantage of the high sensitivity of an electron capture detector to alkyltin halides, an analytical method has been developed for the simultaneous determination of trialkyltin homologues in biological materials. Trialkyltins were purified as chlorides from tissues by simultaneous extraction with hydrochloric acid and ethyl acetate, replacement of the extraction solution with n-hexane and stepwise elution with n-hexane-ethyl acetate on a silica gel column. Alternatively, gas chromatographic analysis was carried out on 20% DEGS-HG at temperatures from 100 to 120 degrees C. Detection limits reached 1 x 10(-12) g for trialkyltin chlorides. The recoveries of trialkyltins added to various tissues at the 50-pmole level ranged from 97 to 106%. By in vivo studies, it was confirmed that this method is rapid, sensitive and applicable to biomaterials containing more than 1 ng trialkyltins per gram of tissue.
利用电子捕获检测器对卤化烷基锡的高灵敏度,已开发出一种同时测定生物材料中三烷基锡同系物的分析方法。通过用盐酸和乙酸乙酯同时萃取,将组织中的三烷基锡以氯化物形式纯化,用正己烷替换萃取液,并在硅胶柱上用正己烷 - 乙酸乙酯进行分步洗脱。或者,在20% DEGS - HG上于100至120摄氏度进行气相色谱分析。三烷基氯化锡的检测限达到1×10⁻¹²克。以50皮摩尔水平添加到各种组织中的三烷基锡的回收率在97%至106%之间。通过体内研究证实,该方法快速、灵敏,适用于每克组织中含有超过1纳克三烷基锡的生物材料。