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
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.0.300 g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0.01~1.0 mg·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10 μg·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.
2-烷基环丁酮
鱼油
固相萃取
GC-MS
2-Alkylcyclobutanones
Fish oil
Solid phase extraction
Abstract
A method of GC-MS for the determination of 2-alkylcyclobutanones,i.e.2-dodecylcyclobutanone and 2-tetradecylcyclobutanone 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-alkylcyclobutanones were kept in the same range of在0.01-1.0 mg·L-1,with lower limits of determination (10S/N) of 10 μg·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%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 “十二五”国家科技支撑计划课题(2012BAD33B02)
收稿日期 2014/5/16
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备注刘茜(1988-),女,山西太原人,硕士研究生,主要研究方向为食品安全检测.
引用该论文: LIU Qian,HAN Li,ZHANG Shu-ya,YI Xiong-hai,DENG Xiao-jun,XI Cun-xian,PENG Tao,LI Wen-bin,DING Zhuo-ping. GC-MS Determination of 2-Alkylcyclobutanones in Irradiated Fish Oil with Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(5): 597～599
刘茜,韩丽,张舒亚,伊雄海,邓晓军,郗存显,彭涛,李文斌,丁卓平. 固相萃取-气相色谱-质谱法测定辐照鱼油中2-烷基环丁酮[J]. 理化检验－化学分册, 2015, 51(5): 597～599
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参考文献
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