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机构地区:[1]中国科学院广州地球化学研究所,广东广州510640 [2]中国科学院大学,北京100049 [3]广州质量监督检测研究院,广东广州510110
出 处:《分析测试学报》2015年第8期874-879,共6页Journal of Instrumental Analysis
基 金:广东省中国科学院全面战略合作项目(2012B090400045)
摘 要:建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定环境水体中呋喃丹、莠去津、甲萘威和6种邻苯二甲酸酯的分析方法。采用Pak C18固相萃取小柱对样品进行富集和净化,甲醇-水为流动相梯度洗脱,以BEH C18柱分离,在串联质谱的多反应监测模式(MRM)下检测,外标法定量。结果表明,在优化实验条件下,9种目标化合物在0.5-20.0μg/L范围内线性关系良好,相关系数均大于0.998,方法检出限(LOD)和方法定量下限(LOQ)分别为0.05-0.12μg/L和0.2-0.3μg/L,回收率为86.0%-96.5%,相对标准偏差(RSD)小于5%。方法快速准确、回收率高,适用于环境水体中呋喃丹、莠去津、甲萘威及6种邻苯二甲酸酯的测定。An analytical method was developed for the simultaneous determination of carbofuran, atrazine, carbaryl and 6 kinds of phthalate esters(PAEs) in environmental water by ultra performance liquid chromatography coupled with tandem quadrupole mass spectrometry ( UPLC - MS/MS). The samples were extracted and purified with Pak C18 solid extraction phase(SPE) cartridge. The targeted compounds were separated on BEH C18 column with methanol water solution as mobile phase , determined under multiple reactions monitoring(MRM) mode and quantified by the external standard method. Under the optimized condition, the calibration curves were linear in the range of 0. 5 -20. 0 μg/ L with correlation coefficients larger than 0. 998. The limits of detection (LOD) and the limits of quantitation(LOQ) of the method were in the ranges of 0. 05 -0. 12 μg/L and 0. 2 -0. 3 μg/L, respectively. The recoveries were between 86. 0% and 96. 5% , with RSDs (n = 6) less than 5%. This method was sensitive, accurate and reliable, and was suitable for the determination of carbofuran, atrazine, carbaryl and 6 kinds of phthalate esters(PAEs) in environmental water.
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