气相色谱—火焰光度法测定大米中三丁基锡和三苯基锡

建立了大米中三丁基锡和三苯基锡化合物同时分析的气相色谱法。样品以二氯甲烷超声提取,四乙基硼酸钠衍生,衍生物经弗罗里硅土层析柱净化后,采用气相色谱—火焰光度法进行检测,并对影响测定的各种因素进行了探讨。三丁基锡、三苯基锡均在0.1~10 mg/L质量浓度范围内线性良好,线性相关系数分别为0.999 0,0.999 5,方法检出限分别为0.049,0.075 mg/kg。在0.5、5.0、10 mg/L 3个添加水平下,三丁基锡、三苯基锡的平均回收率为96.4%~109.4%,相对标准偏差为4.09%~8.46%。方法用于大米中三丁基锡和三苯基锡化合物的同时检测,结果良好。

Determination of Tributyltin and Triphenyltin in Rice by Gas Chromatography-Flame Photometry

A method for simultaneous determination of tributyltin(TBT) and triphenyltin(TPhT) in rice by GC-FPD was developed in this study.The sample was extracted with CH2Cl2 by ultrasonic and derivatived with NaBEt4,then cleaned up by a column filled with florisil.After that,the extract was determined by GC-FPD,the various factors influencing analysis results were explored.The results present the good linearities between analytical signal and analyte concentration in the range of 0.1～10 mg/L with the linear correlation coefficients of 0.9990,0.9995,respectively.For TBT and TPhT,the method detect limit was 0.049 mg/kg and 0.075 mg/kg,respectively.The average recoveries obtained from samples spiked with standards at the concentration levels of 0.5 mg/L,5.0 mg/L and 10 mg/L was in the range of 96.4%～109.4% with relative standard derivation of 4.09%～8.46%.A satisfactory result was obtained in the determination of organotin compounds in rice.