气相色谱法测定白酒中甲基锡及乙基锡

Determination of Methytin and Ethyltin in Chinese Liquor by Gas Chromatography-Flame Photometry

对白酒中的有机锡化合物采用四乙基硼酸钠进行衍生,液-液萃取,应用气相色谱-火焰光度法进行分析,建立白酒样品中二甲基锡、三甲基锡和三乙基锡同时分析新方法。二甲基锡、三甲基锡和三乙基锡的线性范围为0.2～2.5mg/L,相关系数分别为0.9992、0.9980和0.9991,检出限分别为0.0161、0.0167、0.0110mg/L。在0.5、2.0mg/L两个添加水平的平均回收率为67.6%～103.5%,相对标准偏差为5.14%～18.46%。该方法用于白酒中有机锡化合物的同时检测,结果较满意。

A new GC-FPD method for the simultaneous determination of dimethylltin （DMT）, trimethyltin （TMT） and triethyltin （TET） in Chinese liquor was developed. Organotins were derivatized with NaBEt4, extracted by liquid-liquid extraction with n-hexane, and analyzed by gas chromatography-flame photometry （GC-FPD）. The developed calibration curve sof DMT, TMT and TET were all linear in the range of 0.2 -- 2.5 mg/L, with correlation coefficients of 0.9992, 0.9980 and 0.9991, respectively. The limits of detection for three organotins were 0.0161, 0.0167 mg/L and 0.0110 mg/L, respectively. The average recovery rates at spike levels of 0.5 mg/L and 2.0 mg/L were in the range of 67.6%-- 103.5% with RSD between 5.14% and 18.46%. This new method has been applied for the determination of organotin compounds in wine with satisfactory results.