The Determination Of Phthalates In Food By GC-MS And LC-MS/MS

Phthalic acid esters(PAEs)which widely used in hundreds of products as food packaging,toys,perfume,wallpaper,cleaner,nail-polish,spray,shampoo and Shower Gel etc.PAEs has migration,which can damage the reproductive system and the nervous systemTherefore,it is necessary to strictly control the residues of PAEs in food.In this paper,11 kinds of food as the matrix,the detections of 24 kinds of PAEs(DMP、DEP、DIBP、DBP、DMEP、BMPP、DEEP、DPP、DHXP、BBP、DBEP、DCHP、DEHP、DPhP、DNOP、DIPP、DINP、DIDP、DPrP、DIPrP、DHP、DAP、DNP、DINOP)were established by gas chromatography-mass spectrometry and liquid chromatography –tandem mass spectrometry,which provided scientific basis for the detections of PAEs in food.Pretreatment conditions were determined: GC-MS method used liquid-liquid extraction and LC-MS/MS method adopted solid-liquid extraction.The alcohol matrix was purified with HLB cartridges and other matrixes were purified with QuEChERS.For alcohol matrix,the enrichment and purification effect of fillers were compared,such as C18,C8,ProElut,PAS and HLB.As a result,the recoveries of 24 kinds of PAEs were 67.3%-89.5% with amphiphile charicteristics HLB filler,which was better than other fillers and suitable for analyzing multiple PAEs at the same time.Therefore we chose HLB as filler.Ethyl acetate determined as the eluting agent.Methanol was used as constant volume solvent for liquid chromatography-tandem mass spectrometry(LC-MS/MS)and Hexane was used for gas chromatography-mass spectrometry(GC-MS).Instrument improvement and condition optimization: For GC-MS,conditions of GC were optimized through choosing the nonpolar TG-5MS capillary column and control temperature condition.In the MS part,the characteristics of 24 kinds of PAEs compounds were optimized by ion and mass parameters.For LC-MS/MS,the detection instruments were modified using a full-adsorption technology,which inserted a chromatographic column between the mixer and the sample injector to absorb some of the PAEs backgrounds existent in the pipes before the injector.The PAEs in the pipeline was effectively adsorbed,which reduced the migration of PAEs in the detection process.The gradient elution process of LC was optimized,and the characteristics of 24 kinds of PAEs compounds were optimized for the part of MS/MS.The limits of quantitation(LOQ)and linearity of determination method.LOQ of DIDP,DINOP,DINP were 0.5 mg/kg and others were 0.1 mg/kg for GC-MS method.LOQ of DAP was 0.01 mg/kg and others were 0.1 mg/kg for LC-MS/MS method.The correlation coefficients were over 0.99 in the linear range for two methods.The recovery rate and precision of 11 kinds of food matrix were tested by adding standard recovery test.As a result,recovery of method was more than 75% and average of RSD was 4%,which meet the requirements of residues analysis.Two kinds of methods were used for analyzing and evaluating the PAEs in 11 kinds of food matrix.It turned out that PAEs was detected in 11 kinds of commercially available foods.