中空纤维膜液相微萃取-气相色谱质谱法快速测定蔬菜汁中15种邻苯二甲酸酯  

Rapid Determination of 15 Kinds of Phthalate Esters in Vegetable Juices by Hollow Fiber-Liquid Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

作　　者：朱莉萍[1] 朱涛[1] 马运平[1] 倪永付[1] 王勇[1] 闫秋成 

机构地区：[1]济宁出入境检验检疫局,济宁272025

出　　处：《分析化学》2013年第7期1019-1024,共6页Chinese Journal of Analytical Chemistry

摘　　要：采用中空纤维膜-液相微萃取结合GC-MS检测蔬菜汁中15种邻苯二甲酸酯。对萃取溶剂、振荡速度、振荡时间进行了优化:在萃取温度为23℃(室温)、搅拌速度为快速、萃取时间为50min的条件下正己烷萃取效果较好;采用DB-5MS石英毛细管柱(30 m×0.25 mm×0.25μm)、气相色谱质谱(EI)进行分离检测。15种邻苯二甲酸酯在此方法条件下的富集倍数在4.2～315.6之间;检出限在0.0001～0.01 mg/L之间。当添加浓度范围在0.05～1 mg/kg时,回收率在71.8%～90.1%之间,RSD为2.1%～18.9%。本方法可用于蔬菜汁中邻苯二甲酸酯的测定。A method has been developed for the simultaneous determination of 15 phthalate esters in vegetable juices by hollow fiber-liquid phase microextraction coupled with gas chromatography-mass spectrometry. The variable experimental conditions such as extraction organic solvent, extraction time, and frequency of agitation were studied. Under the conditions of room temperature （23℃ ） , fast speed of agitation frequency, extraction time with 50 min, and hexane as the extraction solvent, the extraction efficiency was higher. After extraction, 1 μL organic solvent was injected into GC-MS （El） with column DB-5 （30 m x 0.25 mm x 0.25 μm）. Under the conditions, concentration factors of 15 phthalate esters were 4.2-315.6, limit of detection were 0. 0001- 0.01 mg/L, the recoveries were 71.8% -90.1% , and the relative standard deviations were 2.1% -18.9%. The method is fast and has high sensitivity for the determination of phthalate esters in vegetable juices.

关 键 词：中空纤维膜液相微萃取 邻苯二甲酸酯 蔬菜汁 气相色谱-质谱联用仪 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]