顶空-固相微萃取／气相色谱-质谱法检测酱油中氨基甲酸乙酯含量  

The Development of Headspace Solid-phase Microextraction and Gas Chromatography-tandem Mass Spectrometry for the Detection of Ethyl Carbamate in Soy Sauce

作　　者：张燕[1] 丰帆[1] 姜小梅[1] 郭天鑫[1] 王硕[1] 

机构地区：[1]食品营养与安全省部共建教育部重点实验室,天津科技大学食品工程与生物技术学院,天津300457

出　　处：《食品与发酵工业》2010年第5期114-119,共6页Food and Fermentation Industries

基　　金：国家“863”计划项目(No.2008BAD91B04)

摘　　要：优化建立了固相微萃取．气相色谱-质谱联用技术（HS—SPME—GC／MS）检测酱油中氨基甲酸乙酯含量的方法。取5mL样品，调节pH值为7．5，70℃水浴，搅拌速率800r／min，平衡时间10min，采用75μm CAR／PDMS萃取纤维头，萃取时间30min，气相进样解吸10min。在此条件下，方法检出限（S／N=3）为1．0μg／L，酱油中氨基甲酸乙酯的回收率在70．56％～129．21％，检测结果的日内RSD为3．69％，日间RSD为8．50％。所建立方法可快速、准确地检测酱油中氨基甲酸乙酯含量。A method of headspace solid-phase micro-extraction combined gas chromatography - tandem mass spectrometry was developed and applied to the determination of ethyl carbamate in soy sauce. 75 μm CAR/PDMS fiber was chosen for extracting the ethyl carbamate from the soy sauce. After 5mL of soy sauce （ adjusted to pH 7.5 ） e- quilibrated 10 min at 70 ℃ under 800 r/min, the CAR/PDMS fiber was inserted into the vial for 30 min then injected into GC-MS for 10 min. Under the extraction conditions, the limit of detection was 1.0 μg/mL. The recoveries of ethyl carbamate in soy sauce were 70.56 % - 129.21%. The precisions （RSD） were 3.69 % （intraday） and 8.50 % （inter day）. The HS-SPME/GC/MS technique is suitable for the fast, reliable and inexpensive determination of ethyl carbamate in soy sauce.

关 键 词：氨基甲酸乙酯 酱油 固相微萃取 

分 类 号：TS264.21[轻工技术与工程—发酵工程]