顶空衍生固相微萃取测定大米中醛类物质  

Analysis of aldehydes in rice using solid-phase microextraction with on-fiber derivatization

作　　者：郝俊光 杨理章[1,2,3,4] 樊伟[1,2] 陆健[2,3,4] 董建军 尹花 余俊红 闫鹏 陈华磊 田玉红 

机构地区：[1]啤酒生物发酵工程国家重点实验室,山东青岛266100 [2]江南大学生物工程学院,江苏无锡214122 [3]江南大学粮食发酵工艺与技术国家工程实验室,江苏无锡214122 [4]江南大学工业生物技术教育部重点实验室,江苏无锡214122

出　　处：《食品工业科技》2014年第9期269-274,共6页Science and Technology of Food Industry

基　　金：国家973项目(2012CB723707);江苏高校优势学科建设工程资助项目

摘　　要：本研究利用顶空衍生固相微萃取气相色-谱质谱建立了定量分析大米中醛类物质的方法。通过研究萃取头、衍生剂量、萃取温度和萃取时间对醛类物质检测的影响，确定了顶空衍生固相微萃取的最佳条件：65μm PDMS／DVB在装有10mL 60mg／L邻-五氟苄基羟胺溶液的项空瓶中40℃吸附衍生试剂20rain，之后萃取头换至装有样品的顶空瓶中40℃衍生萃取80min。所建方法的9种醛类物质在各自线性范围内标准曲线线性良好，R2均大于0．99，相对标准偏差在5．0％～7．5％（n=5），检出限在0．010-0．695μg/kg，加标回收率在77．9％～124．2％。本方法可依次自动完成萃取头的衍生试剂吸附以及醛类物质萃取、进样、分离和测定，检测效率高，适用于大米醛类物质的日常大量检测。对大米样品的醛类物质和品评结果进行相关性分析．发现戊醛和己醛是评价大米品盾的重要指标．A simple, practical and sensitive method based on solid-phase micro-extraction （SPME）with on-fiber derivatization coupled with gas chromatography mass spectrometry（GC-MS）was developed for the analysis of aldehydes in rice.The major factors which affect the effect of SPME, such as type of the fiber, quantity of derivatization reagent,temperature and time of extraction were studied.The results showed that a 65 μm PDMS/DVB fiber coating with the 10mL 60mg/L O- （2,3,4,5,6- pentafluorobenzyl） - hydroxylamine for 20min at 40℃ in the headspace of derivatization-reagent-vial followed by extracting for 80min at 40℃ in sample vial headspace was the optimum condition of SPME with on-fiber derivatization.The 9 aldehydes were found to be linear in the validated range with correction coefficients （ R2 ） better than 0.99.The limitations of detection of the method were 0.010-0.695μg/kg in rice while the relative standard deviations （RSD）were 5.0%-7.5% （n = 5）.The recoveries of aldehydes were found to be 77.9% - 124.2%.This consecutive operation of this method, namely coating with the derivatizing reagent,extraction of aldehydes,injection and detection, could automatically completed on line, which made it efficient and suitable for routine analysis of rice aldehydes.Base on correlation anlysis between aldehydes and sensory evaluation scores of rice samples, it was found that hexanal and pentanal were important indices to rice quality.

关 键 词：衍生顶空 固相微萃取 气相色谱质谱 醛类物质大米 

分 类 号：TS207.3[轻工技术与工程—食品科学]