GC-MS/MS法检测并确证纺织品中5种有机锡化合物

Determination and Confirmation of Five Organotin Compounds in Textiles by Gas Chromatography Tandem Mass Spectrometry

建立了气相色谱-串联质谱法(GC-MS/MS)检测和确证纺织品中5种有机锡(一丁基锡、二丁基锡、三丁基锡、二辛基锡、三苯基锡)的快速有效方法。样品经提取、衍生和正己烷液液萃取后,以GC-MS/MS选择反应监测模式(SRM)进行定性定量测定。结果表明,方法在0.02～0.50 mg/L范围内线性关系良好(r>0.999);5种有机锡化合物的定量下限(S/N≥10)为0.03～0.05 mg/kg;加标水平为0.05～0.5 mg/kg时,5种不同材质阴性样品(棉布、真丝、涤纶、羊毛布、棉/尼混纺)的平均回收率为82%～110%,相对标准偏差(RSD,n=5)为2.1%～7.5%。所建立的方法具有选择性强、灵敏度高、定性定量准确等优点,可以弥补气相色谱法(GC)和气相色谱-质谱法(GC-MS)在确证方面的不足,也弥补了液相色谱-串联质谱法(LC-MS/MS)只能检测三取代基有机锡化合物的局限性。

A rapid and effective method was developed for the determination and confirmation of five organotins,including n-butyltin-trichloride（MBT）,dibutyltin-dichloride（DBT）,chlorotributyl-stannane（TBT）,Di-n-octyldichlorotin（DOT） and triphenyltin（TPhT）,in textiles by gas chromatography tandem mass spectrometry（GC-MS/MS）.The target compounds were extracted,derivatized and liquid-liquid extracted with hexane.The qualitative and quantitative analyses were carried out by GC-MS/MS under selected reaction monitoring（SRM） mode.The test result showed that five organotins had good linear relationships（r0.999） between 0.02 mg/L and 0.50 mg/L.The limit of quantitation（LOQ,S/N≥10） of five organotins were between 0.03 mg/kg and 0.05 mg/kg.At the spiked levels of 0.05-0.5 mg/kg in five kinds of negative samples（e.g.cotton,real silk,wool,polyester and cotton/nylon）,the average recoveries of five organotins were in the range of 82%-110%,with relative standard deviations（RSD,n=5） of 2.1%-7.5%.With high sensitivity,selectivity and good precision and accuracy,this established method could make up the shortage of confirmations by GC and GC-MS,and was suitable for the determination of different structures of organotin compounds such as mono-substituted,di-substituted and tri-substituted organotin compounds etc.,compensating for the limitation of the LC-MS/MS method which could only detect tri-substituted organotin compounds.