固相萃取-气相色谱-质谱法测定辐照鱼油中2-烷基环丁酮  

GC-MS Determination of 2-Alkylcyclobutanones in Irradiated Fish Oil with Solid Phase Extraction

作　　者：刘茜[1] 韩丽[2] 张舒亚[2] 伊雄海[2] 邓晓军[2] 郗存显[3] 彭涛[4] 李文斌 丁卓平[1] 

机构地区：[1]上海海洋大学食品学院,上海201306 [2]上海出入境检验检疫局,上海200135 [3]重庆出入境检验检疫局,重庆400020 [4]中国检验检疫科学研究院,北京100123 [5]迪马公司,天津300400

出　　处：《理化检验（化学分册）》2015年第5期597-599,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金："十二五"国家科技支撑计划课题(2012BAD33B02)

摘　　要：提出了固相萃取-气相色谱-质谱法测定辐照鱼油中2-烷基环丁酮（2-十二烷基环丁酮和2-十四烷基环丁酮）含量的方法。0.300g辐照鱼油样品用正己烷溶解,ProElut Silica固相萃取柱净化。在气相色谱分离中用HP-5MS色谱柱为固定相,在质谱分析中采用选择离子监测模式。2种2-烷基环丁酮的质量浓度均在0.01~1.0mg·L-1范围内与其峰面积呈线性关系,方法的测定下限（10S/N）为10μg·kg-1。加标回收率在91.2%~96.0%之间,测定值的相对标准偏差（n=6）在3.7%~5.9%之间。A method of GC-MS for the determination of 2-alkylcyclobutanones, i.e. 2-dodecylcyclobutanone and 2-tetradecylcyelobutanone in irradiated fish oil with solid phase extraction was proposed. The sample （0. 300 g） of irradiated fish oil was dissolved with n-hexane, and cleaned up with a ProElut Silica solid phase extraction column. The HP-5MS chromatographic column was used for GC separation and the selected ion monitoring mode was adopted in MS determination. Linear relationships between values of peak area and mass concentration of the two 2-alkylcyelobutanones were kept in the same range of 在0. 01 - 1. 0 mg·L-1 , with lower limits of determination （10S/N） of 10g·kg-1. Values of recovery found by standard addition method were in the range of 91.2%--96. 0%, with RSD＇s （n=6） in the range of 3. 7%-5.9%.

关 键 词：气相色谱-质谱法 2-烷基环丁酮 鱼油 固相萃取 

分 类 号：O657.63[理学—分析化学]