固相微萃取-气相色谱/串联质谱在线酯交换测定啤酒原料的亚油酸甘油酯  

Determination of glyceryl linoleate in malt and rice for brewing by gas chromatography-tandem mass spectrometer with simultaneous transesterification and solid-phase micro-extraction

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

机构地区：[1]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 [2]啤酒生物发酵工程国家重点实验室(筹),山东青岛266061 [3]江南大学工业生物技术教育部重点实验室,江苏无锡214122 [4]江南大学生物工程学院,江苏无锡214122

出　　处：《食品工业科技》2013年第20期60-64,共5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：利用固相微萃取气相串联质谱(SPME-GC-MS/MS)在线酯交换建立了定量分析啤酒原料(麦芽和大米)的亚油酸甘油酯的方法。通过研究不同因素对酯交换及萃取效果的影响,确定在线酯交换固相微萃取的最佳条件:2.0mL样品稀释液添加0.75mL氢氧化钾/甲醇(10.7mmol/L)和1.0g氯化钠,用85μmPA萃取头在65℃下酯交换和萃取60min。为降低基体效应对定量准确性的影响,以三亚油酸甘油酯为外标分别建立了麦芽和大米的标准曲线。该方法在麦芽和大米中检出限为0.132、0.579μg/g,三亚油酸甘油酯加标回收率为116%和114%。此方法相比于传统方法,所需样品量少、准确性高、操作过程简便,适用于啤酒原料的亚油酸甘油酯的日常高效检测。A method based on solid-phase micro-extraction（SPME） with simultaneous transesterification coupled with gas chromatography-tandem mass spectrometry（GC-MS/MS） was developed for the determination of glyceryl linoleate in raw materials（malt and rice） for beer. The impact of different factors on transesterification and extraction was investigated. The results showed that a 851Jm Polyacrylate fiber extracting for 60min at 65℃ after adding 0.75 mL 10.7mmol/L KOH/CH3OH and lg NaCI in sample diluents was the best choice. The matrix effect was reduced by spiking glyceryl trilinoleate as an external standard in malt and rice,respectively. The limitations of detection of the method were 0.132μg/g in malt and 0.579μg/g in rice. The recoveries of glyceryl trilinoleate were found to be 116% and 114% at the spike levels of 5.0mg/g and 1.0mg/g in malt and rice matrices, respectively. Comparing to traditional way,the advantages of this method were less sample needed ,accuracy simple operation process and suitability for routine analysis of glyceryl linoleate in raw materials for beer.

关 键 词：在线酯交换 固相微萃取 气相色谱串联质谱 啤酒原料 亚油酸甘油酯 

分 类 号：TS207.3[轻工技术与工程—食品科学]