摘要
建立了固相萃取-高效液相色谱-质谱法测定水体中11种三嗪类除草剂的方法.通过全自动固相萃取和浓缩增加环境样品的富集倍数,将定容好的样品经过液相色谱分离,采用质谱检测离子对,以保留时间定性,离子对定量.对方法条件进行优化,并检测了长江支流的实际水样.结果表明,样品冷藏避光可保存7 d,不用调节pH值,用HLB固相萃取柱萃取,用乙腈作为洗脱溶剂,11种三嗪类除草剂的相关系数为0.997～0.999,检出限为0.010～0.021 ng/L,加标回收率为61.3％～106％,相对标准偏差为3.91％～9.37％.宜昌境内长江支流的水样有莠去津等7种三嗪类除草剂被检出,其余4种未检出.该方法具有较低的检出限,较好的准确度和精密度,适用于地表水中三嗪类除草剂的检测.
Abstract
A method was developed for detection of 11 triazine herbicides.After automatic solid-phase extraction and concentration,the extracts were separated by liquid chromatography and detected by mass spectrometry.Qualification was done according to retention time and quantitation was carried out by ion-pair.The method conditions were optimized before testing real samples from branch of the Yangtz River.The results showed that samples can be refrigerated in darkness for 7 d,HLB cartridge is suitable for extraction of target compounds from water samples without adjusting pH value with acetonitrile as elution solvent.The correlation coefficients of 11 triazine herbicides were 0.997～0.999.The detection limits of 11 triazine herbicides were 0.010～0.021 ng/L.The average recovery rates of 11 triazine herbicides were 61.3％～106％.The precision ranged from 3.91％～9.37％.Seven types of triazine herbicides including atrazine were detected in Yichang section of the Yangtze River tributaries,while no other triazine herbicides were detected.The method has a low detection limit,good accuracy and precision,and is suitable for the detection of triazine herbicides in surface water.
基金项目
三峡库区生态环境教育部工程研究中心开放基金(KF2022-03)
NETL
NSTL
万方数据