分散固相萃取-气相色谱-质谱法测定含油脂食品中17种邻苯二甲酸酯

Determination of 17 Phthalic Acid Esters in Fatty Food by Dispersive Solid Phase Extraction-Gas Chromatography-Mass Spectrometry

建立了含油脂食品中17种邻苯二甲酸酯的分散固相萃取-气相色谱-质谱法检测方法。奶茶样品经乙腈-甲基叔丁基醚(9∶1,V/V)提取后,提取液用MAS-PAEC分散固相萃取管进行净化。调味包样品经乙腈(正己烷饱和)-甲基叔丁基醚(19∶1,V/V)提取2次后,提取液用CNW分散固相萃取管进行净化。采用基质匹配标准外标法进行定量分析。结果表明,奶茶中17种邻苯二甲酸酯的加标回收率为82.2%～125.4%;相对标准偏差小于16.5%;方法检出限为100～200μg/L。调味包中17种邻苯二甲酸酯的加标回收率为70.9%～115.5%;相对标准偏差小于9.8%;方法检出限为400～800μg/L。本方法快速、精确、简易、廉价、稳定,可应用于含油脂食品中17种邻苯二甲酸酯的实际检测分析。

A method was developed for the determination of 17 phthalic acid esters in fatty food by dispersive solid phase extraction-gas chromatography-mass spectrometry（d-SPE-GC-MS）.Tea milk samples were extracted with acetonitrile： methyl tert-butyl ether（9 ∶ 1,V/V）,and the extract was cleaned up by MAS-PAEC d-SPE column.Flavor seasonings samples were extracted with acetonitrile（saturated with hexane）： methyl tert-butyl ether（19 ∶ 1,V/V）,and the extract was cleaned up by CNW d-SPE column.Matrix-match external standard method was used for quantification.The results showed that the average recoveries of 17 phthalic acid esters in milk tea were 82.2%-125.4% and relative standard deviations were less than 16.5%.The limit of detection（LOD） of all the compounds were 100-200 μg/kg.The average recoveries of 17 phthalic acid esters in flavor seasonings were 70.9%-115.5% and relative standard deviations were less than 9.8%.The limits of detection（LOD） of all the compounds were 400-800 μg/kg.The method is quick,sensitive,easy,cheap,rugged,and can be applied to the detection of 17 phthalic acid esters in fatty food.