A novel method for the determination of vanillin in powdered milk by liquid-liquid extraction - solidification of acceptor phase droplet-reextraction combined with gas chromatography/mass spectrometry(GC/MS) was developed. The sample was extracted with ether and the supernatant was cleaned up using 0.01 mol/L 100 μL sodium hydroxide and the residue was reextracted with dichloromethane. The detection of vanillin was carried out by GC—MS in selected ion monitoring(SIM) mode and external standard method was used for quantitative determination. Under the optimum conditions, the linear range of the method was from 0.20 to 10.0 μg/mL and the linear correlation coefficient (R) was higher than 0.999 5. The limit of detection (S/N=3) was 0.004 mg/kg. The relative standard deviation of the method was less than 6.83% with the recovery values ranging from 82.0% to 98.0%. The proposed method which is very simple, rapid and highly sensitive can meet the needs of determination of vanillin in powdered milk.

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