分散液液微萃取-高效液相色谱法测定白酒中的酞酸酯  

Determination of Phthalate Esters in White Spirits by Dispersive Liquid-Liquid Microextraction Combined with High Performance Liquid Chromatography

作　　者：曹江平[1] 范盈盈[1] 解启龙[1] 白玮玮[1] 刘书慧[1,2] 张晓科[3] 

机构地区：[1]西北农林科技大学理学院,陕西杨凌712100 [2]旱区作物逆境生物学国家重点实验室,陕西杨凌712100 [3]西北农林科技大学农学院,陕西杨凌712100

出　　处：《食品科学》2013年第24期233-237,共5页Food Science

基　　金：西北农林科技大学人才专项(Z111021005)

摘　　要：建立分散液液微萃取（DLLME）-高效液相色谱法（HPLC）测定白酒中邻苯二甲酸二异丁酯（DIBP）、邻苯二甲酸二丁酯（DBP）和邻苯二甲酸丁苄酯（BBP）的方法。考察萃取剂和分散剂的类型及体积、盐离子强度、萃取温度和萃取时间对萃取效率的影响。2mL样品溶液加入7mL0．26g／mLNaCI溶液稀释后，加入预先混匀的60此四氯化碳（萃取剂）和60此乙腈（分散剂），室温轻摇5min，离心后用进样针吸取离心管底部四氯化碳沉积相，用等体积甲醇稀释进样。方法的线性范围为1-500ng／mL（r〉0．99），检测限为0．3～0．8ng／mL（RSN=3）；富集倍数为92～102；重复性良好，日内及日间重复测定的相对标准偏差分别为1．3％～2．8％、2．0％～4．7％（n=6）。将该法应用于31种市售白酒中酞酸酯的测定，含量分别为DIBP：0．01～5．35μg／mL；DBP：0．01～7．60μg／mL；BBP：0．0l～0．07μg／mL。17种不同品牌白酒中DBP的含量超标。加标回收率为92．5％～111．2％。该方法具有有机溶剂用量少、操作简单快捷、灵敏度高等优点。A novel method for the determination of diisobutyl phthalate （DIBP）, dibutyl phthalate （DBP） and butyl benzyl phthalate （BBP） in white spirits has been developed by using dispersive liquid-liquid microextraction （DLLME） coupled with high performance liquid chromatography with a DAD detector. Key DLLME experimental parameters including the type and volume of extractant and disperser solvent, the amount of added salt, extraction time and temperature were examined and optimized. The optimized extraction conditions were as follows： 2 mL of sample diluted with 7 mL of 0.26 g/mL NaC1 solution and then mixed with a pre-mixed solution consisting of 60 IxL of carbon tetrachloride （extractant） and the same volume of acetonitrile （disperser solvent） by gently shaking for 5 min at room temperature. After centrifugation, the precipitate phase of carbon tetrachloride was taken and diluted with the same methanol before being injected into the analytical column for analysis. The method revealed an excellent linearity over the concentration range of 1-500 ng/mL with correlation coefficient （r） 〉 0.99. The detection limits were in the range of 0.3-0.8 ng/mL. The enrichment factors varied from 92 to 102. Intra-day and inter-day repeatability values expressed as relative standard deviation were in the range of 1.3%-2.8%, and 2.0%-4.7% （n = 6）, respectively. The developed method was applied to the determination of the phthalate esters in 31 white spirits, and 17 out of the detected samples exceeded the legal limit of DBP. The average recovery rates ranged from 92.5%-111.2%. Compared to previous methods, the new procedure is characteristics of simple sample preparation, less organic solvent consumption and higher sensitivity.

关 键 词：分散液液微萃取 白酒 酞酸酯 

分 类 号：TS207.3[轻工技术与工程—食品科学]