摘要
为准确检测地下水等环境水体中痕量草甘膦等有机磷化合物的含量,服务水环境质量评价,通过优化色谱条件、样品预处理及定量方法选择等方面的讨论,建立了离子色谱-串联质谱法测定水样中5种有机磷化合物(草甘膦、草铵膦、氨甲基膦酸、杀木磷、乙烯利)的分析方法。水样经微孔滤膜过滤,通过稀释或阳离子交换柱进行预处理。以Ion Pac AS11-HC(250 mm×2 mm)为分离柱,KOH溶液为淋洗液进行梯度洗脱,串联质谱的多反应监测模式分析,内标法定量。结果表明,5种有机磷化合物的线性关系良好(r>0.999),检出限在0.006~0.1μg/L之间。在地表水、地下水和工业废水的加标回收率为74.0%~130%,相对标准偏差在2.9%~8.8%之间。该方法操作简单、快速、灵敏、准确,与标准方法《水质草甘膦的测定高效液相色谱法》(HJ1071-2019)进行方法比对研究,测定结果无显著性差异。同时,在方法建立的过程中,对可能存在的基质干扰及消除进行了探讨,可以通过调整色谱条件、稀释样品或减少进样量、阳离子交换柱的预处理和内标法定量来降低和补偿基质干扰。
In order to accurately detect trace amounts of glyphosate and other organophosphorus compounds in groundwater and other environmental water,and to serve the environmental quality evaluation of water,through the discussion on the optimization of chromatographic conditions,sample pretreatment and quantitative methods,an ion chromatography-tandem mass spectrometry method was developed for the determination of five organophosphorus compounds(glyphosate,glufosinate,aminomethylphosphonic acid,fosamine and ethephon)in water samples.The water samples were filtered by microporous membrane and were pretreated by dilution or cation exchange column.The separation of organophosphorus compounds was performed on an Ion Pac AS11-HC(250 mm×2 mm)by gradient elution using KOH solution,the detection was achieved by tandem mass spectrometry in multiple reaction monitoring mode,and quantitative by internal standard method.The results showed that the calibration curves of five organophosphorus compounds had good linearity(the correlation coefficients>0.999)and the detection limits ranged from 0.006 to 0.1μg/L.The average recoveries and relative standard deviation of organophosphorus compound in surface water,underground water and waste water were 74.0%~130%and 2.9%~8.8%.The method was simple,rapid,sensitive and accurate,and compared with the standard method"Determination of glyphosate in water quality by high performance liquid chromatography"(HJ1071-2019),the results showed no significant difference.During the development of this method,the possible matrix interference and its elimination were discussed.The matrix interference can be reduced and compensated by adjusting chromatographic conditions,diluting the sample or reducing the amount of sample injection,pretreatment of cation exchange column and quantification by internal standard method.
作者
赵云芝
王若男
朱红霞
宋望
ZHAO Yun-zhi;WANG Ruo-nan;ZHU Hong-xia;SONG Wang(Sichuan Ecological and Environmental Monitoring Center,Chengdu 610091,China;China National Environmental Monitoring Centre,Beijing 100012,China;Sichuan Mianyang Ecological and Environmental Monitoring Center,Mianyang,Sichuan 621000,China)
出处
《四川环境》
2022年第6期26-32,共7页
Sichuan Environment
关键词
有机磷化合物
离子色谱-串联质谱法
水样
方法比对
基质干扰
Organophosphorus compounds
ion chromatography-tandem mass spectrometry
water sample
methods comparison
matrix interference
