建立小体积液液萃取-气相色谱-三重四极杆串联质谱法测定地下水中32种半挥发性有机污染物(SVOCs)的方法.采用2 mL二氯甲烷和正己烷混合溶剂(体积比为1∶1)加入到20 mL水样中,添加2 g NaCl,涡旋萃取60 s,经DB-5MS UI色谱柱(30 m×0.25 mm,0.25 μm)分离,SRM模式检测,内标法定量.32种SVOCs的质量浓度在0.5~20 μg/L范围内与色谱峰面积具有良好的线性关系,相关系数均大于0.995,方法检出限为0.002~0.06 μg/L.样品加标回收率为72.5%~129%,测定结果的相对标准偏差为0.65%~21.1%(n=6).该方法样品处理简单快捷,所需水样和有机试剂体积较少,能够满足地下水中32种SVOCs的高效测定.
A method for the determination of 32 semi-volatile organic pollutants(SVOCs)in groundwater by small volume liquid-liquid extraction gas chromatography-triple quadrupole tandem mass spectrometry was established.A mixed solvent of 2 mL dichloromethane and n-hexane(volume ratio of 1∶1)was added to 20 mL water sample,and 2 g NaCl was added.After vortex extraction for 60 s,the sample was separated by DB-5MS UI chromatographic column(30 m×0.25 mm,0.25 μm),detected by SRM mode,and quantified by internal standard method.The mass concentration of 32 SVOCs had a good linear relationship with the chromatographic peak area in the range of 0.5-20 μg/L,the correlation coefficients were all more than 0.995,and the detection limit of the method was 0.002-0.06 μg/L.The spiked recoveries of the samples were 72.5%-129%,and the relative standard deviations of the determination results were 0.65%-21.1%(n=6).The method is simple and fast in sample processing,requires less water samples and organic reagents,and can meet the efficient determination of 32 SVOCs in groundwater.