响应面优化HS-SPME-GC/MS检测啤酒微量酯类物质条件  

Optimization of HS-SPME-GC/MS conditions for determination of trace esters in beer by response surface method

作　　者：许杨 王德良[1] 李红[1] 闫寅卓[1] 宋涛[1] 

机构地区：[1]中国食品发酵工业研究院,北京100015

出　　处：《中国酿造》2017年第9期163-167,共5页China Brewing

基　　金：国家自然科学基金(31401680)

摘　　要：该研究采用Plackett-Burman和Box-Behnken试验设计,对顶空固相微萃取-气相色谱-质谱法(HS-SPME-GC/MS)检测啤酒中6种低含量酯类物质(辛酸乙酯、丁酸乙酯、乙酸异丁酯、乙酸苯乙酯、苯甲酸乙酯和3-苯基丙酸乙酯)的萃取条件进行优化,发现萃取温度、萃取时间和平衡温度为主要影响因素,通过响应面法分析得出最佳萃取条件为:萃取温度42℃、萃取时间30 min和平衡温度48℃;在该条件下,结合内标法定量,该方法的相关系数R2为0.990 0~0.999 9,回收率为93.43%~103.37%,检测限为0.01~0.05μg/L,相对标准偏差(RSD)为1.75%~8.24%,表明该方法准确可靠,可应用于啤酒中微量酯类物质的检测。The six low-content esters （including ethyl caprylate, ethyl butyrate, isobutyl acetate, phenylethyl acetate, ethyl l^nzoate and ethyl 3-phenylpropi- on） were extracted and determined by headspace solid-phase microextraction and gas chromatography-mass spectrometry （HS-SPME-GC/MS）. The extrac- tion conditions were optimized by Plackett-Burman and Box-Behnken experiments. The result showed that extraction temperature, extraction time and equilibrium temperature were identified as the main factors. Through response surface methodology analysis, the optimum extraction conditions were temperature 42 ＇12, time 30 min and equilibrium temperature 48 ℃. Under the conditions, combined with the internal standard method to quantify, the RE of the method was 0.990 0-0.999 9, the recovery rate was 93.43%-103.37%. The limit of detection was 0.01-0.05 μg/L. The relative standard deviation （RSD） was 1.75%-8.24%, which indicated that the method was accurate and reliable, and could be applied to the determination of trace esters in beer.

关 键 词：啤酒 微量酯类物质 顶空固相微萃取.气相色谱质谱法 响应面法 检测分析 

分 类 号：TS261.7[轻工技术与工程—发酵工程] O657.63[轻工技术与工程—食品科学与工程]