Abstract:

A method for the determination of dicyandiamide in milk was developed by syncore analyst/ultra performance
liquid chromatography-electrospray ionization tandem mass spectrometry (SA-UPLC-MS-MS). Deuterium substituted
reagents were used as internal standards and added to the sample before extraction. The mixture 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
limit of detection (LOD) for dicyandiamide were 10 μg/kg, and limit of quantitation (LOQ) were 50 μg/kg. The correlation
coefficient of the linear calibration curve was over 0.990 within the dicyandiamide concentration range 10–1000 ng/mL. The
average recoveries for dicyandiamide were 99.6% to 102.3% (n = 6). The proposed method is simple, rapid, reliable, stable
and sensitive. It can meet the requirements for the determination of dicyandiamide in milk.

Key words: ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-MS-MS), syncore analyst (SA), dicyandiamide, milk