分散液液微萃取-气相色谱法测定复杂食品基质中对羟基苯甲酸酯类  

Determination of p-hydroxy Benzoates in Complex Food Matrix Using Dispersive Liquid-Liquid Microextraction/Gas Chromatography

作　　者：何浩 陈幸莺 梁林富 钟鹏鹏 蔡永 孙映球 赵娟 

机构地区：[1]湘潭市食品药品检验所,湖南湘潭411100 [2]中南林业科技大学,湖南长沙410004

出　　处：《食品研究与开发》2017年第23期146-150,共5页Food Research and Development

基　　金：湖南省食品药品监督管理局食品药品安全科技项目(R201715)

摘　　要：建立复杂食品基质中对羟基苯甲酸酯类及其钠盐的分散液液微萃取(Dispersive Liquid-Liquid Microextraction,DLLME)-气相色谱(Gas Chromatography,GC)检测方法。样品浸泡在水中,经煮沸和超声两个步骤提取目标物质。取4 mL待测液,调节p H后分别加入0.6 g氯化钠,0.3 mL四氯化碳和0.6 mL丙酮,手动和涡旋萃取,离心后取下层有机相分析,外标法定量。该方法在25 mg/kg^1 000 mg/kg范围内线性良好,r2为0.997 2~0.999 0,回收率为95.6%~99.2%,相对标准偏差均小于4.0。对羟基苯甲酸甲酯、乙酯、丙酯和丁酯的定量下限为1.2 mg/kg^3.2 mg/kg。A dispersive liquid liquid microextraction(DLLME)and gas chromatographic(GC)method for the determination of p-hydroxy benzoates and its salts in complex food matrix was established. Sample was soaked in water,using boiling and ultrasound two steps to extract the target material. Take 4 mL sample solution,after adjusting p H,0.6 g sodium chloride,0.3 mL carbon tetrachloride and 0.6 mL acetone were added. Using manual and vortex extraction,after centrifugation,the organic phase was analyzed. The linearity was good in 25 mg/kg-1 000 mg/kg using this method,r2 was 0.997 2-0.999 0,the recovery rate was 95.6 %-99.2 %,the relative standard deviation was less than 4.0. The lower limit of quantification for methyl,ethyl,propyl,butyl paraben was 1.2 mg/kg-3.2 mg/kg.

关 键 词：分散液液微萃取 气相色谱法 对羟基苯甲酸酸酯类 复杂食品基质 

分 类 号：O657.71[理学—分析化学] TS207.3[理学—化学]