啤酒中邻苯二甲酸酯的GC-MS测定

Analysis of phthalates in beer by GC-MS

采用气相色谱-质谱联用法(GC-MS)测定啤酒样品中邻苯二甲酸酯(PAEs)。研究表明:用Na Cl和超声波协助正己烷萃取样品中PAEs,可有效提高PAEs萃取效率和消除乳化现象,同时可将萃取液直接进行GC-MS测定,建立了干扰性小、重现性好、快速简便的啤酒样品中PAEs残留量的测定方法。在该分析条件下,12种PAEs标准曲线均有良好的线性(其中DMP、DEP、DIBP、DBP、BMPP、DPP、DHXP、BBP、DEHP的线性范围是5~500μg/L,DMEP、DCHP和DPHP的线性范围是10~500μg/L,线性相关性为0.995 7<R2<0.999 7)。3个质量浓度梯度(25、50、125μg/L)的平均回收率在88.21%~110.11%,相对标准偏差(RSD,n=6)在0.40%~5.49%。

The phthalates( PAEs) in beer were analyzed by GC / MS method in this study. The results revealed that Na Cl addition and ultrasound in extracting PAEs from beer sample using n-hexane enhanced extraction efficiency and eliminated emulsification effectively. A method for residual PAEs determination in beer was developed,which was simple,quick,accurate and reproducible. Under the analytical conditions,12 PAEs had good linearity( in the range of 5 ~ 500 μg / L for DMP,DEP,DIBP,DBP,BMPP,DPP,DHXP,BBP,DEHP and 10 ~ 500 μg / L for DMEP,DCHP and DPHP) with the correlation coefficient( R2) varying from 0. 995 7 to 0. 999 7. The average recoveries of three concentrations( 25,50,125 μg / L) reached 88. 21% ~ 110. 11% with the relative standard deviation( RSD,n= 6) of 0. 40% ~ 5. 49%. This method was successfully applied in the determination of PAEs in 20 commercially available beer samples and reliable results were obtained. The method developed in this study is sensitive,simple,accurate and quick,which meets the demand of PAEs determination in beer.