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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 被引量:61

Determination of 17 Phthalic Acid Esters in Fatty Food by Dispersive Solid Phase Extraction-Gas Chromatography-Mass Spectrometry
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摘要 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.
出处 《分析化学》 SCIE CAS CSCD 北大核心 2012年第3期391-396,共6页 Chinese Journal of Analytical Chemistry
基金 湛江出入境检验检疫局科研项目(No.2011/003)资助
关键词 分散固相萃取 气相色谱-质谱 含油脂食品 邻苯二甲酸酯 Dispersive solid phase extraction Gas chromatography-mass spectrometry Fatty food phthalic acid esters
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