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目的:建立一种牛奶和奶粉中氯霉素残留量的超高效液相色谱质谱检测方法。方法:采用冷冻高速离心分离脂肪和沉淀部分蛋白,用乙酸乙酯提取,正己烷脱脂,C18固相萃取柱净化,甲醇洗脱,氮气吹干。用超高效液相色谱-串联质谱仪测定,外标法定量。结果:在0.05μg/L～2.0μg/L范围内,线性良好,相关系数为0.999601(n=5)。加标回收率在90%～110%,相对标准偏差在10%以内。最低检出限为0.05μg/L(kg)。结论:本方法操作简便,检出限低,重复性好,达到了国家标准要求,适合牛奶中氯霉素残留测定。
Objective: To establish a method for the determination of chloramphenicol residues in milk and milk powder by ultra performance liquid chromatography-mass spectrometry. Methods: Freezing fat and precipitating some proteins by freeze-high speed centrifugation, extracting with ethyl acetate, defatting with n-hexane, purifying with C18 solid phase extraction column, eluting with methanol and blowing dry with nitrogen. Using ultra performance liquid chromatography - tandem mass spectrometry, external standard method. Results: The linearity was good in the range of 0.05μg / L ~ 2.0μg / L with a correlation coefficient of 0.999601 (n = 5). Spike recovery of 90% to 110%, the relative standard deviation of less than 10%. The minimum detection limit of 0.05μg / L (kg). Conclusion: The method has the advantages of simple operation, low detection limit, good repeatability, meeting the requirements of national standards and being suitable for the determination of chloramphenicol residues in milk.