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目的:建立一种要儿配方奶粉中双氰胺残留量的超高效液相色谱质谱检测方法。方法:采用三氯乙酸溶液沉淀蛋白,处理液用Waters Sep-Pak AC2固相萃取柱净化,用超高效液相色谱-串联质谱仪测定,外标法定量。结果:在0.10μg/mL~50.0μg/mL范围内,线性良好,线性方程为y=2310.43×x+1.01815,相关系数为0.999826(n=6)。加标回收率在90%~110%,相对标准偏差在10%以内。最低检出限为0.05mg/kg。结论:本方法操作简便,检出限低,重复性好,适合婴儿配方奶粉中双氰胺残留的测定。
Objective: To establish a method for the determination of dicyandiamide residues in infant formula milk powder by ultra performance liquid chromatography-mass spectrometry. Methods: The trichloroacetic acid solution was used to precipitate the protein. The treatment solution was purified with Waters Sep-Pak AC2 SPE cartridge and quantified by ultra performance liquid chromatography-tandem mass spectrometry. Results: In the range of 0.10μg / mL ~ 50.0μg / mL, the linearity was good and the linear equation was y = 2310.43 × x + 1.01815 with a correlation coefficient of 0.999826 (n = 6). Spike recovery of 90% to 110%, the relative standard deviation of less than 10%. The minimum detection limit is 0.05mg / kg. Conclusion: The method is simple, low detection limit, good reproducibility, suitable for the determination of dicyandiamide residues in infant formula.