建立了高效液相色谱-串联质谱检测农产品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HPLC-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40μg/kg。在10~1 000 ng/mL内峰强度与质量浓度的线性关系良好(r>0.999)。方法的平均回收率在94.8%~103.3%。

The method for determination of dicyandiamide in farm products was developed by performance liquid chromatography-electrospray ionization tandem mass spectrometry( HPLC-MS / MS). Deuterium substituted reagent were used as internal standards and added to the sample before extraction. The sample was extracted with aminated acetonitrile,concentrated with syncore analyst,and cleaned up by hexane. The mass spectrometer was operated in the positive ion mode using select reaction monitoring for qualitative and quantitative analysis of dicyandiamide. The limits of detection for dicyandiamide were 10 μg / kg and limits of quantization were 40 μg / kg. The correlation coefficient of linear calibration curve was over 0. 999 within the dicyandiamide concentration range 10 ~ 1000ng / ml. The average recoveries for dicyandiamide were 94. 8% to103. 3%. The method is simple,rapid,reliable,stable and sensitive. It can meet the requirements of the daily work for the determination of dicyandiamide in agriculture products.