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建立了浊点萃取-超高效液相色谱分析(CPE-UPLC)法测定水中戊菌唑残留量的方法。以非离子表面活性剂PEG-6000为萃取剂,对色谱检测条件和浊点萃取参数进行了探讨和优化。浊点萃取条件为27 g/L PEG-6000,120 g/L Na2SO4,溶液p H为1.5,在45℃水浴中平衡15 min。在选定的色谱条件下,戊菌唑在0.025~5.0μg/m L时其质量浓度与检测信号峰面积呈线性关系,相关系数为0.9997,检出限为1.5μg/L;水样平均添加回收率为91.4%~92.9%,相对标准偏差为1.8%~2.6%。水样中戊菌唑添加质量浓度(0.025~5.0μg/m L)经CPE处理与UPLC检测信号呈线性关系,相关系数为0.9979,检出限为0.2μg/L,方法能满足农药残留检测的要求。
A method of cloud point extraction-ultra performance liquid chromatography (CPE-UPLC) was established for the determination of penicillazole residues in water. With non-ionic surfactant PEG-6000 as extractant, the chromatographic conditions and cloud point extraction parameters were discussed and optimized. Cloud point extraction conditions for the 27 g / L PEG-6000, 120 g / L Na2SO4, the solution p H was 1.5, in a 45 ℃ water bath for 15 min. Under the selected chromatographic conditions, the concentration of penconazole in the range of 0.025 ~ 5.0μg / m L showed a linear relationship with the detection signal peak area, the correlation coefficient was 0.9997, the detection limit was 1.5μg / L; The recoveries ranged from 91.4% to 92.9% with relative standard deviations of 1.8% -2.6%. The concentration of penconazole added in water samples (0.025 ~ 5.0μg / m L) was linearly correlated with the UPLC signal by CPE, the correlation coefficient was 0.9979, the detection limit was 0.2μg / L, and the method could meet the requirements of pesticide residue detection Claim.