CAJ | 학술논문

建立了顶空固相微萃取-气相色谱-质谱(HS-SPME-GC-MS)结合邻-五氟苄基羟胺(PFBHA)衍生以测定啤酒中与老化味相关的13种醛类化合物的方法.样品前处理不同于文献报道的方法,衍生试剂直接加入到啤酒样品中,然后插入SPME装置,一步完成衍生和萃取过程.经优化的固相微萃取条件为:65μm PDMS/DVB萃取头,萃取温度50℃,萃取时间60 min.GC-MS分析采用选择离子模式(SIM)并以内标法定量,所建方法的定量重复性较好,样品重复测定的RSD在2.5%-19.5%;回收率在55.3%-108.8%.在测定新鲜和老化啤酒时,显示出该方法具有较好的适用性.
건립료정공고상미췌취-기상색보-질보(HS-SPME-GC-MS)결합린-오불변기간알(PFBHA)연생이측정비주중여노화미상관적13충철류화합물적방법.양품전처리불동우문헌보도적방법,연생시제직접가입도비주양품중,연후삽입SPME장치,일보완성연생화췌취과정.경우화적고상미췌취조건위:65μm PDMS/DVB췌취두,췌취온도50℃,췌취시간60 min.GC-MS분석채용선택리자모식(SIM)병이내표법정량,소건방법적정량중복성교호,양품중복측정적RSD재2.5%-19.5%;회수솔재55.3%-108.8%.재측정신선화노화비주시,현시출해방법구유교호적괄용성.
A method for the determination of 13 stale-flavor aldehydes in beer was developed with o-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine(PFBHA) derivation by Headspace Solid Phase Microextraction (HS-SPME) and GC-MS analysis. Different from the former studies, derivation and extraction process were performed in one step as the deriving reagent was directly added in beer sample and SPME fiber was then exposed into the sample vial. The opti-mized SPME conditions were at 50℃ for 60min with 65um PDMS/DVB fiber. GC-MS analysis was achieved by SIM mode using E-2-heptenal as internal standard. The method was shown good repeatability with RSD between 2. 5%-19.5% and the recoveries were ranged from 55.3 to 108.8%. The method was successfully applied to fresh and aged beer with good applicability.