摘要
A new method for simultaneous determination of four phthalate esters ( PAEs) in commercial fat-containing foods was developed by the combination of a packed nanofibers column based on solid-phase extraction with gas chromatography-flame ionization detector ( GC-FID ). Conditions for obtaining optimum extraction efficiency such as extraction solvents, morphologies of adsorbent, ion strength and pH were investigated and optimized in detail. Under the optimized conditions, the limits of detection (LODs) found for dibutyl phthalate (DBP) , butyl benzyl phthalate (BBP), diethyl hexyl phthalate (DEHP) and di-n-octyl phthalate (DNOP) were 50, 25, 50 and 25 ng/g, respectively. Good linearity of four PAEs was achieved in the range of 50 to 4 000 ng/g. The proposed method was applied for analyzing different kinds of fat-containing samples. PAEs in commercial fat-containing samples can be highly extracted by a packed solid-phase extraction column of 5 mg polystyrene ( PS) nanofibers. The satisfactory average recoveries were obtained in the range of 96. 7% to 102. 3% , and the relative standard deviations (RSDs) below 5% were achieved. The proposed method reduces the organic solvent consumption, the complex and tedious procedures for sample pretreatment, and achieves high sensitivity and reproducibility for the investigated PAEs.
将纳米纤维固相萃取技术与气相色谱-火焰离子化检测器相结合,建立了同时检测油脂类食品中4种邻苯二甲酸酯(邻苯二甲酸二丁酯( DBP)、邻苯二甲酸丁基苄酯( BBP)、邻苯二甲酸-(2-乙基己)酯(DE- HP)、邻苯二甲酸二正辛酯( DNOP) )的新方法.为了获得最佳提取效率,对提取条件包括提取溶剂、吸附剂 形貌、离子强度和pH进行了优化.在最佳提取条件下, DBP, BBP, DEHP和 DNOP的检出限分别为50,25, 50,25 ng/ g,线性范围为50-4 000 ng/ g.将该方法应用于多种食用油样品的检测,只需5mg PS纳米纤维, 即可实现油脂类食品中PAEs的高效萃取,回收率为96 .7 % - 102.3%,相对标准偏差(RSD)小于5 % .该方 法减少了有机溶剂的使用量和样品前处理过程中复杂繁琐的程序,灵敏度高,重现性好.
基金
The National Basic Research Program of China(973Program)(No.2012CB933302)
the National Instrumental Research Program(No.2014YQ06077303)
the National Natural Science Foundation of China(No.81172720,21307086)
Suzhou Science and Technology Department Foundation(No.ZXG201441)