Abstract:

A method for the analysis of sixteen phthalate acid ester (PAE) residues in health wine was developed using gas chromatography-triple quadrupole mass spectrometry (GC-QQQ-MS). The health wine samples were extracted with n-hexane by liquid-liquid extraction method before analysis. The samples were detected by GC-QQQ-MS with electron impact source (EI) in selected ion monitoring (SIM) mode after extraction. The separation was performed on an HP-5MS capillary column (30 m×0.25 mm×0.25 μm) with temperature programming. The retention time and the fragment ion abundance ratio were used to judge the qualitative results, and the quantitation was performed with standard curve method of the characteristic ion chromatographic peak area-concentration. Eighty-one batches of health wine samples were detected using the method. The results showed that the method had good linear relationships with correlation coefficients (r²) not less than 0.9959. The recoveries of fifteen PAEs ranged from 88.6% to 107.3% except dimethyl phthalate (DMP) which was 52.3%-58.7% in all the three spiked levels with the relative standard deviations of 0.1%-6.8%(RSD, n=6). The limits of detection were between 0.002 mg/L to 0.061 mg/L. The limits of quantification were between 0.005mg/L and 0.202 mg/L. The method is accurate, sensitive, proprietary and suitable for the simultaneous determination of the sixteen phthalate acid esters in health wine.

Key words: gas chromatography-mass spectrometry (GC-MS), health wine, phthalate acid esters (PAEs), plasticizer