人造革合成革中的中链和短链氯化石蜡的测定——气相色谱-负化学离子源质谱法

Determination of MCCPs and SCCPs in Leatherette by GC-ECNI-MS

建立了使用气相色谱-电子捕获负化学离子源质谱法(GC-ECNI-MS)同时测定人造革合成革产品中的中链和短链氯化石蜡含量的检测方法。人造革合成革样品经正己烷在50℃下超声萃取60 min,再经过浓硫酸净化后,采用GC-ECNI-MS进行测试,内标法定量。中短链氯化石蜡通过总体响应因子校正法定量,线性相关系数均大于0.99。短链氯化石蜡的空白样品加标回收率为88.4%~95.7%,相对标准偏差为1.5%~3.0%;中链氯化石蜡的空白样品加标回收率为88.3%~103.2%,相对标准偏差为1.6%~6.9%。检出限为5 mg/kg,定量限位17 mg/kg,可满足人造革合成革中的中链和短链氯化石蜡的测定要求。

A method was developed for the simultaneous determination of medium-chain chlorinated paraffins(MCCPs)and short-chain chlorinated paraffins(SCCPs)in leatherette by GC-ECNI-MS.Leatherette samples were ultrasonically extracted with n-hexane at 50℃for 60 min,then purified with concentrated sulfuric acid,tested by GC-ECNI-MS,and quantified by internal standard method.MCCPs and SCCPs were quantified by the total response factor correction method,and the linear correlation coefficients were>0.99.The recoveries of blank samples of SCCPs ranged from 88.4%to 95.7%with relative standard deviations of 1.5%-3.0%.The recoveries of blank samples of MCCPs ranged from 88.3%to 103.2%with relative standard deviations of 1.6%-6.9%.The detection limit is 5 mg/kg,and the quantitative limit is 17 mg/kg,which can meet the requirements for the determination of MCCPs and SCCPs in leatherette.