An efficient and simple method for determining vanillin, methyl vanillin and ethyl vanillin in milk and dairy products was developed using a liquid-liquid extraction (LLE) procedure coupled to high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). Different extraction procedures were tested and optimised by spiking three vanillin compounds into a blank matrix in which none of any food additives were detected, and the extraction with acetonitrile solution and n-hexane as cleaning sorbent allowed an efficient recovery of 87.6-101.7% with RSDs less than 5%. The limit of detection (LOD) ranged from 6.2 to 20.1 μg/kg. High sensitivity, accuracy and selectivity were found for the in-house validated method, which can eliminate the interferences from complicated matrices effectively, and fulfil the quality criteria for routine laboratory application for real samples. The developed method was then finally applied to screen the three analytes in 65 milk and dairy products including infant formula milk powders from local markets to check for compliance with Chinese Regulation. Concentrations of the total vanillin and ethyl vanillin ranged from 0.0323 to 246.3 mg/kg, which is within the limits of Chinese regulations.
Keywords: Vanillin; dairy products; flavours; high performance liquid chromatography tandem mass spectrometry; milk.