尼龙6纳米纤维膜固相萃取-液相色谱法测定食用油中邻苯二甲酸酯

Determination of Phthalates Esters in Edible Oil by High Performance Liquid Chromatography with Solid-membrane Extraction Based on Electrospun Nylon 6 Nanofibrous Membrane

建立了溶剂提取、尼龙6（PA6）纳米纤维膜萃取净化,液相色谱-紫外法（HPLC-UV）检测食用油样品中5种邻苯二甲酸酯的方法。对洗脱溶剂的种类及用量、纳米纤维膜的用量、pH值、突破体积及过样速度等影响因素进行了考察。在最优化条件下,邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二乙酯（DEP）、邻苯二甲酸二丁酯（DBP）、邻苯二甲酸二异辛酯（DEHP）和邻苯二甲酸二正辛酯（DOP）的检出限分别为0.020,0.030,0.080,0.100和0.150ng/mL,相对标准偏差（RSD）为5.3%～7.0%,回收率为85.9%～101.0%。将该方法应用于实际样品的检测,只需2.5mgPA6纳米纤维膜,即可完成对样品中的PAEs的萃取,方法精密度与回收率与相关文献方法相当,而检出限更低。

A new method was developed for the simultaneous determination of five phthalate esters in oil samples by a combination of mat-based solid-phase extraction （SPE） with high performance chromatography. The mat was composed of polyamide 6（PA6） nanofibers. Dimethyl phthalate （DMP） edible liquid diethl phthalate （ DEP）, di-n-butyl phthalate （ DBP）, di- （2-ethylhexyl） phthalate （DEHP） and dioctyl phthalate （DOP） were successfully separated on a RP-Cls column. Under the optimum conditions, the detection limits of DMP, DEP, DBP, DEHP and DOP were 0. 020-0. 150 ng/mL. Spiked samples gave recoveries in the range from 85.92% to 101.03%, with relative standard deviations 5.3% -7.0%. The proposed method only required much lower consumption of organic solvent and sorbents, and gave lower detection limits than the methods in the literatures, and with comparative precision and accuracy.