摘要
本研究建立了固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)测定水中16种有机磷农药残留的分析方法。考察了C18柱和HLB柱分别串联活性炭AC固相萃取柱的萃取效果,以及单一和混合溶剂的洗脱效果。水样用0.45μm滤膜过滤后用HCl调节pH至4,经HLB-活性炭AC串联小柱富集净化后,分别用丙酮-二氯甲烷(4∶1,V/V)和5 mmol/L NH 4Ac甲醇溶液洗脱HLB小柱和活性炭AC小柱,洗脱液混合氮吹复溶,定容后采用外标法定量分析。在最佳测试条件下,16种目标物在1~100μg/L范围内呈现良好的线性关系,相关系数(R 2)均大于0.991,检出限为0.004~0.238 ng/L;平均回收率在55.5%~109.7%之间,相对标准偏差(RSD)为2.0%~13.9%。该方法灵敏度较高,重复性好,适用于水中16种有机磷农药残留检测。
A method was established for the detection of 16 kinds of organophosphorus pesticides in water by ultra-high performance liquid chromatography-tandem mass spectrometry with solid-phase extraction(SPE-UPLC/MS/MS).The extraction efficiency of C18-AC and HLB-AC tandem SPE columns and the elution efficiency of single and mixed solvents were compared.The water sample filtered by 0.45μm filter membrane was adjusted to pH=4 with hydrochloric acid,enriched and cleaned-up by HLB-AC tandem SPE column,then respectively eluted by ethyl dichloromethane-acetone(1∶4,V/V)and 5 mmol/L ammonium acetate methanol solution.The mixture of eluents dried with nitrogen flow and reconstituted,subsequently quantified by external standard method.Under the optimal conditions,the calibration curves of the 16 compounds showed good linearity in the range of 1-100μg/L with the correlation coefficients(R 2)larger than 0.991.The limits of detection ranged from 0.004 to 0.238 ng/L.The average recoveries of samples were 55.5%-109.7%with relative standard deviations of 2.0%-13.9%.This method has the advantages of good sensitivity and reproducibility and could be applied in the detection of the 16 organophosphorus pesticides in water.
作者
高振刚
曾莎莎
曾鸿鹄
梁延鹏
覃礼堂
宋晓红
GAO Zhengang;ZENG Shasha;ZENG Honghu;LIANG Yanpeng;QIN Litang;SONG Xiaohong(College of Environmental Science and Engineering,Guilin University of Technology,Guilin 541004;Guangxi Key Laboratory of Environmental Pollution Control Theory and Technology,Guilin University of Technology,Guilin 541004;Collaborative Innovation Center for Water Pollution Control and Water Safety in Karst Area,Guilin University of Technology,Guilin 541004)
出处
《分析科学学报》
CAS
CSCD
北大核心
2021年第1期22-28,共7页
Journal of Analytical Science
基金
国家自然科学基金(No.51868012,51578171)
广西科技计划(桂科AD18126018)
广西“八桂学者”岗位专项经费资助。
关键词
固相萃取
超高效液相色谱-串联质谱
有机磷农药
Solid-phase extraction
Ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry
Organophosphorus pesticide
