摘要
利用固相萃取-超高效液相色谱(UHPLC)-四极杆-飞行时间质谱(Q-TOF/MS)法建立了26种农药的快速筛查和检测方法.首先建立了包含26种农药的一级精确质量数及保留时间、二级离子谱库的数据库.通过谱库信息比对,可实现地表水中26种农药的无标准品的情况下定性鉴定.样品经过C18萃取小柱富集、净化,用乙腈-异丙醇(1∶1,V/V)洗脱.采用C18色谱柱分离,0.1%甲酸甲醇溶液(含10 mmol·L^-1乙酸铵)和0.1%甲酸水溶液(含10 mmol·L^-1乙酸铵)进行梯度洗脱,再利用UHPLC-Q-TOF/MS检测,外标法定量.结果表明,在线性范围内,26种农药的线性关系良好,线性相关系数≥0.994,加标回收率在67.74%-112.3%之间,相对标准偏差(RSD)0.45%-12.2%之间.
A rapid method for the screening and determination of 26 pesticides was developed based on solid phase extraction and ultrahigh performance liquid chromatography(UHPLC)-quadrupole time-of-flight mass spectrometry(Q-TOF/MS). Initially, a database containing the accurate mass, retention time and the MS/MS spectra of the 26 pesticides was established. Based on the above database, the qualitative identifications of the 26 pesticides in surface water were accomplished without comparison with the standard substances. The target compounds in real water samples were first enriched by solid phase extraction cartridges and then eluted out of the cartridges using acetonitrile/isopropanol solution(1∶1). The resultant samples were then loaded onto a reversed phase C18 column and subjected to separation under gradient elution using 0.1% formic acid in methanol and 0.1% formic acid in water(with 10 mmol·L^-1 ammonium acetate) as binary mobile phases, further detected using UHPLC-Q-TOF/MS, and quantificated by external standard method. It was demonstrated that in the studied concentration range, all 26 pesticides exhibited very good linearity with the linear correlation coefficients all higher than 0.994. The recoveries ranged from 67.74% to 112.3% with the relative standard deviations(RSD) between 0.45% and 12.2%.
作者
赖国银
林立毅
丁亦男
曹淑瑞
袁文萱
徐敦明
严丽娟
吴敏
吕美玲
LAI Guoyin;LIN Liyi;DING Yinan;CAO Shurui;YUAN Wenxuan;XU Dimming;YAN Lijuan;WU Min;LYU Meiling(Technical Center of Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen, 361026, China;The Inspection Technical Center of Chongqing Entry-Exit Inspection & Quarantine Bureau, Chongqing, 400020, China;Agilent Technologies (China) Co., Ltd, Beijing, 100102, China)
出处
《环境化学》
CAS
CSCD
北大核心
2019年第5期1065-1073,共9页
Environmental Chemistry
基金
国家重点研发计划(2017YFC1601606)
福建省自然科学基金(2016J05045)资助~~
