Determination of phthalate esters in Chinese spirits using isotope dilution gas chromatography with tandem mass spectrometry

Phthalate esters are additives used in polyvinylchloride and are found as contaminants in many food products. An isotope dilution mass spectrometry technique has been developed for accurate analysis of 16 phthalate esters in Chinese spirits by adopting the 16 corresponding isotope-labeled phthalate esters. The ethanol in the spirit sample was first removed by heating with a water bath at 100°C with a stream of nitrogen, after which the residue was extracted with n-hexane twice. The phthalates collected were identified and quantified by gas chromatography with tandem mass spectrometry in multiple reaction monitoring mode. The spiking recoveries of 16 analytes ranged from 94.3 to 105.3% with relative standard deviation values of <6.5%. The detection limits for 16 analytes were <10.0 ng/g. The expanded relative uncertainties were from 3.0 to 14%. A survey was performed on Chinese spirits from the market. Six of the nine analyzed samples were contaminated by phthalates. Di-n-butyl phthalate and di-2-ethylhexyl phthalate showed higher detection frequency and concentrations. This isotope dilution gas chromatography with tandem mass spectrometry method is simple, rapid, accurate, and highly sensitive, which qualifies as a candidate reference method for the determination of phthalates in spirits.