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建立超高效液相色谱-串联质谱(UPLC-MS-MS)检测奶粉中双氰胺残留量的检测方法。以氘代试剂为内标,样品经氨化乙腈萃取后,平行定量浓缩仪浓缩,用正己烷脱脂,采用UPLC-MS-MS选择反应监测(SRM)正离子模式测定。双氰胺的检出限可达10μg/kg,最低定量限可达50μg/kg。在10~1000ng/mL范围内峰强度与质量浓度的线性关系良好(r>0.990)。方法的平均回收率在99.6%~102.3%之间。方法简单、快速、稳定、准确、灵敏度高,能够满足日常工作中奶粉双氰胺的检测要求。
To establish a method for the determination of dicyandiamide residues in milk powder by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS). Using deuterated reagent as internal standard, the sample was extracted with ammoniated acetonitrile and concentrated in a parallel quantitative concentrator. The sample was defatted with n-hexane and determined by UPLC-MS-MS selective reaction monitoring (SRM). Detection limit of dicyandiamide up to 10μg / kg, the minimum limit of quantification of up to 50μg / kg. The linear relationship between peak intensity and mass concentration ranged from 10 to 1000 ng / mL (r> 0.990). The average recoveries of the method ranged from 99.6% to 102.3%. The method is simple, rapid, stable, accurate and sensitive, and can meet the detection requirements of dicyandiamide milk powder in daily work.