气相色谱-质谱法测定纺织助剂中的有机锡

Determination of organotin compounds in textile auxiliaries by gas chromatography-mass spectrometry

建立了纺织助剂中二丁基锡（d ibu ty ltin,DBT）、三丁基锡（tribu ty ltin,TBT）及三苯基锡（tripheny ltin,TPhT）化合物的气相色谱-质谱联用（gas ch rom a tography-m ass spec trom etry,GC-M S）检测方法。在乙酸-乙酸钠缓冲溶液（pH4.0）中,用正己烷超声萃取（对疏水性样品）或振荡萃取（对亲水性样品）试样中的有机锡,然后以四乙基硼化钠的四氢呋喃溶液为衍生化试剂进行衍生化,用GC-M S测定,依据保留时间和选择离子定性,外标法定量。实验结果表明,在0.1~8.0m g/L（对于DBT和TBT）或0.1~4.0m g/L（对于TPhT）的范围内,有机锡化合物的浓度（以有机锡阳离子计）与其衍生物峰面积呈良好的线性关系,线性相关系数（r2）为0.999 4~0.999 8,检出限为0.003~0.005m g/L;4种聚氨酯类助剂基质中3种有机锡化合物的平均加标回收率为92.6%~108.0%,相对标准偏差为2.5%~10.2%。该方法的技术指标满足纺织助剂中有机锡化合物的测定要求。

A gas chromatography-mass spectrometry（GC-MS） method has been developed for the determination of dibutyltin（DBT）,tributyltin（TBT） and triphenyltin（TPhT） in textile auxiliaries.The sample was first extracted with n-hexane in acetate buffer solution（pH 4.0） under ultrasonication（for hydrophobic sample） or oscillation extraction（for hydrophilic sample） and then derivatized with sodium tetraethylborate in tetrahydrofuran.The derivative was determined by GC-MS in selected ion monitoring（SIM） mode.The separation and quantification were achieved using a Rxi-5ms silica capillary column（30 m×0.25 mm×0.25 μm）.The linear ranges were 0.1-8.0 mg/L for both DBT and TBT,and 0.1-4.0 mg/L for TPhT.There were good linear relationships between the peak area and concentration in the linear ranges and the correlation coefficients（r2） were 0.9994-0.9998.The detection limits（LOD） were from 0.003 mg/L to 0.005 mg/L.The average recoveries of these organotin compounds at the three spiked levels of 4.0,10.0 and 40.0 mg/kg were 92.6%-108.0% with the relative standard deviations（RSDs） of 2.5%-10.2%.The method is simple and accurate for simultaneous analysis of the DBT,TBT and TPhT in textile auxiliaries.