摘要
建立了固相萃取水中6种邻苯二甲酸酯类化合物,结合气相色谱质谱法定性定量分析的方法,并将其应用于实际水样的监测。比较了硅胶柱、C18、Qasis HLB和Si/PSA玻璃柱对6种PAEs回收率的影响。结果表明,Si/PSA玻璃柱回收率最稳定,平均回收率在92.5%~102.3%之间,Qasis HLB次之,回收率在85.9%~104.7%之间,C18的回收率为76.7%~88.3%,硅胶柱的回收率为71.8%~102.1%。水样加入经Si/PSA玻璃小柱富集净化,用乙腈洗脱后浓缩近干,用正己烷定容至1mL,采用内标法定量。6种PAEs在20.0~500.0μg·L^-1浓度范围内线性关系良好,相关系数均大于0.998,在3个加标水平下,回收率在89.4%~99.6%之间,精密度在1.11%~4.75%之间,方法检出限均低于0.2μg·L^-1。采用该方法分析6个实际水样中的PAEs,发现所有水样中均有邻苯二甲酸酯类物质残留,回收率在85.9%~101.3%。该法回收率稳定,抗干扰能力强,灵敏度高,适用于水中痕量PAEs的批量监测。
The method for the determination of six kinds of phthalates esters(PAEs)in surface water by solid-phase extraction combined with GCMS was established.In this paper,extraction efficiency of PAEs by four SPE colums(Silica,C18,Qasis HLB and Si/PSA)was compared.The results showed that the Si/PSA was the most suitable SPE with the recoveries range from 92.5%to 102.3%.Followed by Qasis HLB with the average recoveries between 85.9%and 104.7%,the C18 from 76.7%to 88.3%,and the Silica SPE showed an unstable recoveries from 71.8%to 102.1%.To evaluate the performance of Si/PSA SPE extraction,validation experiments were carried out on water samples at three spiking levels.Water sample was enriched and purified by Si/PSA SPE,eluted by acetonitrile,then the elution solution was nearly dried and finally diluted to 1.0 mL with hexane and determined by GCMS and quantified with internal standard.The result showed that the calbration curves were linear in the range of 20.0~500.0μg·L^-1 for target compounds,with correlation coefficients above 0.998.Meanwhile,the recoveries were in the range of 89.4%~99.6%,and the relative standard deviation(RSD)were in the range of1.11%~4.75%,the limits of detection(LODs)for all five chlorobenzenes were below 0.2μg·L^-1.In addition,PAEs in different water sources were determined by Si/PSA SPE-GCMS,the result showed that the recoveries was between 85.9%and 101.3%,which could better complete the task of water quality monitoring in advantage of its stable extrction efficiency,strong anti-interference ability and high sensitivity.
作者
张少倩
ZHANG Shao-qian(Nanyang Eco-environment Bureau,Nanyang 473000,China)
出处
《化学工程师》
CAS
2019年第12期28-31,共4页
Chemical Engineer
关键词
邻苯二甲酸酯
水
气相色谱
phthalates esters(PAEs)
water
gas chromatography
