引用本文:陈冠焱,张兆年,宋环宇,金德周,张珊,谭颖喆,王晶晶.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[J].环境监控与预警,2024,(3):54-58
CHEN Guanyan,ZHANG Zhaonian,SONG Huanyu,JIN Dezhou,ZHANG Shan,TAN Yinzhe,WANG Jingjing.Determination of 11 Triazine Herbicides in Water by Solid Phase Extraction-High Performance Liquid Chromatography-Mass Spectrometry[J].Environmental Monitoring and Forewarning,2024,(3):54-58
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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
陈冠焱1,张兆年1,宋环宇2,金德周1,张珊1,谭颖喆2,王晶晶1
1.湖北省生态环境厅宜昌生态环境监测中心,湖北 宜昌 443000; 2. 宜昌市三峡库区生态环境监测站,湖北 宜昌 443000
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。
关键词:  固相萃取  高效液相色谱-质谱法  水体  三嗪类除草剂
DOI:DOI:10.3969/j.issn.1674-6732.2024.03.009
分类号:X832
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课题(KF2022-03)
Determination of 11 Triazine Herbicides in Water by Solid Phase Extraction-High Performance Liquid Chromatography-Mass Spectrometry
CHEN Guanyan1, ZHANG Zhaonian1, SONG Huanyu2, JIN Dezhou1, ZHANG Shan1, TAN Yinzhe2, WANG Jingjing1
1.Yichang Ecological Environment Monitoring Center of Hubei Provincial Department of Ecological Environment, Yichang, Hubei 443000, China; 2.Yichang Three Gorges Reservoir Ecological Environment Monitoring Station, Yichang, Hubei 443000, China
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.
Key words:  Soild phase extraction  High performance liquid chromatography mass spectrometry  Water  Triazine herbicides