A QuEChERS with high performance liquid chromatographic ( HPLC) method was developed for the determination of 17 phthalate esters ( PAEs), e.g. DMEP, DMP, DEEP, DEP, DPhP, BBP, DIBP, DBP, DBEP, DPP, DCHP, BMPP, DHXP, DEHP, DNOP, DINP and DNP, in food samples. The targeted compounds were extracted with acetonitrile, and purified by PSA-based QuEChERS (50 mg PSA and 150 mg MgSO4). The extract were separated on a Ci8 column with mobile phase composed of water and acetonitrile by gradient elution at a flow rate of 1. 0 mL/min. The UV detection wavelength was set at 224 nm. Under the optimal conditions, the calibration curves of phthalate esters were linear in the ranges of 0. 5 - 10 mg/L for DINP and 0. 05 - 10 mg/L for the others with correlation coefficients ( r ) more than 0. 99. The average recoveries of 17 analytes from 5 kinds of food matrixes were in the range of 70% - 120% with RSDs ( n = 6 ) less than 15% . The detection limits ( LODs, S/N = 3 ) of phthalate esters were 0. 001 - 0. 02 mg/L and the quantitation limits (LOQs, S/N = 10) were 0. 05 - 0. 5 mg/kg. The proposed procedure was applied in the analysis of 432 real samples from Xiamen, Fujian province( China) , in which 18 positive samples were found. The proposed method was simple and accurate, and could be applicable for the routine analysis of monitoring PAEs residues in foodstuffs.%建立了同时检测食品中17种邻苯二甲酸酯类化合物的QuEChERS/高效液相色谱分析方法.样品经乙腈提取,采用含50 mg PSA和150 mg MgSO4填料的净化管进行净化,分析液经C18柱分离,乙腈-水为流动相梯度洗脱,流速1.0 mL/min,紫外检测波长224 nm.在优化色谱条件下,DINP在0.5～10 mg/L范围内,其余16种分析物在0.05 ～ 10 mg/L范围内线性关系良好,仪器检出限(LOD,S/N=3)为0.001 ～0.02mg/L,方法的定量下限(LOQ,S/N=10)为0.05 ～0.5 mg/kg.对调味精粉、葡萄果冻、凤梨酥、鸡蛋面、柚子酱5种食品中17种分析物的加标回收率为70％ ～ 120％,相对标准偏差(RSD)小于15％.该方法稳定、可靠,可满足食品中邻苯二甲酸酯类化合物的检测需要.
展开▼
