Determination of Vanillin and Ethyl-Vanillin in Milk Powder by Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

A method for determination of vanillin and ethyl-vanillin in milk powder by auto headspace solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was established. Vanillins in sample were extracted with SPME through a fused-silica fiber coated with divinylbenzene/polydimethylsiloxane. The analytes were desorbed by GC at 260 °C for 5 min and separated on a DB-5MS capillary column and detected by MS with EI source by selected ion monitoring mode (EI-SIM). As a result, the limit of detection of vanillin and ethyl-vanillin was 0.1 and 0.05 mg/kg. The spiked recovery was between 90.0 and 100 %, and the RSD ranged from 1.9 to 5.1 % (n = 6). This method eliminated the interferences from complicated matrix effectively. The method was successfully applied for quick determination of vanillin and ethyl-vanillin content in milk powder samples.