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作 者:何书海[1,2] 曹小聪[1,2] 吴海军 李腾崖 张鸣珊[1,2] 陈表娟[1,2] HE Shu-hai;CAO Xiao-cong;WU Hai-jun;LI Teng-ya;ZHANG Ming-shan;CHEN Biao-juan(Hainan Province Environmental Monitoring Centre,Haikou 571126,China;Hainan Province Research Academy of Environmental Sciences,Haikou 571126,China;SCIEX,Guangzhou 510000,China)
机构地区:[1]海南省环境监测中心站,海口571126 [2]海南省环境科学研究院,海口571126 [3]SCIEX公司,广州510000
出 处:《农药》2019年第10期741-744,共4页Agrochemicals
摘 要:[目的]建立了一种简便、直接进样的超高效液相色谱-三重四级杆质谱法(UPLC-MS/MS)快速测定地表水和地下水中阿维菌素的残留。[方法]水质样品经甲醇等体积稀释,用0.22μm滤膜过滤去除杂质后,滤液直接进行定量分析。阿维菌素通过KINETEX C18柱分离,以乙腈-2.5 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,在正离子模式下以MRM方式进行检测。[结果]阿维菌素在0.10~20.0μg/L范围内线性关系良好,相关系数(r)大于0.999,方法检出限为0.02μg/L。实际水质样品在低、中、高3种加标质量浓度下,回收率分别为96%~98%、98%~100%和100%~101%,相对标准偏差分别为5.6%~7.4%、4.5%~5.1%、1.8%~2.8%。[结论]该方法操作简便,灵敏度高,准确性高,重现性好,实现了4 min内完成水质中痕量阿维菌素的分析。[Aims] A method was established for the rapid determination of abamectin in surface water and ground water by direct injection-ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLCMS/MS). [Methods] The water samples were diluted with equal volume of methanol and were filtered with 0.22 μm filter membrane to remove impurities. Then the quantitative analysis of the filtrates was conducted through UPLC-MS/MS. The analytes were separated on a KINETEX C18 column with gradient elution using mobile phases of acetonitrile containing 2.5 mmol/L ammonium acetate aqueous solution. The data were collected by positive electrospray ionization in the multiple reaction monitoring(MRM) mode. [Results] The correlation coefficients(r) of linear calibration curve were over 0.999 in the corresponding linear ranges(0.10-20.0 μg/L). The method limit of detection was 0.02 μg/L. The recovery rates of the abamectin were in the range of 96-98, 98-100 and 100-101% at the low,medium and high spike levels, respectively. [Conclusions] The corresponding relative standard deviations were in the range of 5.6-7.4, 4.5-5.1 and 1.8-2.8%, respectively. The detection method is simple, sensitive, accurate, reliable and suitable for the detection of trace level of abamectin in water within 4 minutes.
关 键 词:超高效液相色谱-三重四极杆质谱 直接进样 阿维菌素 环境水样
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