摘要
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,0.25μm)分离,SRM模式检测,内标法定量。32种SVOCs的质量浓度在0.5~20μg/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0.002~0.06μg/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,0.25μm),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 0.5-20μg/L,the correlation coefficients were all more than 0.995,and the detection limit of the method was 0.002-0.06μg/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.
作者
周宇齐
钟旭
宋洲
罗火焰
卢显鹏
吉义平
ZHOU Yuqi;ZHONG Xu;SONG Zhou;LUO Huoyan;LU Xianpeng;JI Yiping(Hubei Province Geological Experimental Testing Center,Wuhan 430034,China;Hubei Huaxiang Geological Environment Testing Technology Co.,Ltd.,Wuhan 430000,China;Hubei Key Laboratory of Resources and Eco-environment Geology(Hubei Geological Bureau),Wuhan 430034,China)
出处
《化学分析计量》
CAS
2024年第1期27-34,52,共9页
Chemical Analysis And Meterage
基金
湖北省地质局科技项目(KJ2021-18,KJ2022-36,KJ2023-39)。
关键词
小体积液液萃取
气相色谱-三重四极杆串联质谱法
半挥发性有机污染物
地下水
small volume liquid-liquid extraction
gas chromatography-triple quadrupole mass spectrometry
semivolatile organic pollutants
groundwater