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建立了婴幼儿奶粉中双氰胺的前处理方法和串联四级杆液质联用分析方法,采用乙腈提取,Sep-pak AC2固相萃取柱净化,超高效液相色谱(UPLC)分离,串联四极杆质谱多反应离子监测,该方法在5~100μg/L的范围内线性关系良好,相关系数(r2)大于0.995,3个浓度的加标回收率为80.8%~88.7%,相对标准偏差为2.2%~3.0%,具有很好的精密度,方法检出限可达到0.3μg/kg。
A pretreatment method of dicyandiamide and tandem quadrupole liquid chromatography-mass spectrometry (LC-MS / MS) methods were established for the determination of dicyandiamide in infant milk powder. The samples were extracted with acetonitrile, purified with Sep-pak AC2 solid phase extraction cartridge, separated by ultra performance liquid chromatography (UPLC) Quadrupole mass spectrometry and multi-reactive ion monitoring. The calibration curve was linear in the range of 5-100 μg / L with a correlation coefficient (r2) of greater than 0.995. The spiked recoveries of the three concentrations ranged from 80.8% to 88.7%, and the relative standard deviations Is 2.2% ~ 3.0%, with good precision, the detection limit of the method can reach 0.3μg / kg.