基于杯[6]芳烃萃取头的固相微萃取-气相色谱法测定啤酒中痕量的酞酸酯类化合物  

Determination of trace phthalates in beer by gas chroma-tography coupled with solid-phase microextraction using a calix[6]arene fiber

作　　者：高洁[1] 杨偲[1] 叶长文[1] 李秀娟[1] 

机构地区：[1]华中农业大学食品科技学院,湖北武汉430070

出　　处：《色谱》2009年第3期356-358,共3页Chinese Journal of Chromatography

基　　金：国家大学生创新性实验计划项目(200834);教育部新教师基金项目(081025)

摘　　要：选用自制杯[6]芳烃溶胶-凝胶固相微萃取(SPME)萃取头,建立了顶空SPME与气相色谱联用检测啤酒中8种酞酸酯(PAEs)的方法。采用L25(56)正交设计对萃取条件进行了优化,所得方法检出限为0.003～3.429μg/L,相对标准偏差不超过13.5%,加标回收率为86.3%～109.3%。采用标准加入法对3种瓶装啤酒中PAEs进行了检测,结果表明邻苯二甲酸二(2-乙基己)酯(DEHP)是啤酒中最主要的酞酸酯类污染物,含量最高达5.24μg/L。迁移试验表明,瓶装啤酒所用塑料垫圈中高含量的DEHP可能成为酒体中PAEs的一种来源,且延长贮存时间、提高贮存温度和振荡都能加快垫圈中DEHP的迁移。A method based on headspace solid-phase microextraction/gas chromatography （HS-SPME/GC） for the determination of phthalates （PAEs） in beer using benzoxy-C[6]/OH-TSO coated fiber was developed. A Taguchi’s L25（5^6） orthogonal array design was employed to evaluate potentially significant factors and screen the optimum conditions for each analyte to ensure the highest extraction efficiency. The extraction for the determination of dimethyl phthalate （DMP） and diethyl phthalate （DEP） was carried out at 65 ℃ for 50 min with a constant stirring speed of 1250 r/min, that of dibutyl phthalate （DBP） and diamyl phthalate （DAP） was at 95 ℃ for 50 min with a speed of 624 r/min, and that of the other PAEs was at 105 ℃ for 60 min without agitation. Owing to the good selectivity and high sensitivity of this new calixarene fiber, the method enabled the quantification of PAEs at low μg/L level in beer media with good precisions and recoveries. The survey of three bottled beer samples showed that DBP and bis（2-ethylhexyl）-phthalate （DEHP） were the main PAEs found in beer and total phthalates concentrations were between 6.22 and 7.76 μg/L. The migration tests revealed that the high content of DEHP incorporated in PVC gaskets in the lids could be a potential source of PAEs contamination in bottled beer during transportation and storage.

关 键 词：固相微萃取 杯芳烃 气相色谱法 酞酸酯类化合物 迁移 痕量分析 啤酒 

分 类 号：O658[理学—分析化学]