双柱分离-气相色谱法测定火锅底料中罂粟碱  

Determination of papaverine in hotpot seasoning by double column separation-gas chromatography

作　　者：范翔[1] 冯家力[1] 陈东洋[1] 丁力[1] 李欣[1] 杨静玥 

机构地区：[1]湖南省疾病预防控制中心,湖南长沙410005

出　　处：《中国卫生检验杂志》2015年第14期2296-2298,2301,共4页Chinese Journal of Health Laboratory Technology

基　　金：湖南省科技厅科技计划课题(2012FJ4106)

摘　　要：目的建立双柱分离-气相色谱法检测火锅底料等食品中罂粟碱的方法。方法样品经正己烷分散油脂后,用盐酸提取其中罂粟碱,并通过移除正己烷以除去样品油脂;盐酸提取液用氢氧化钠调至碱性,再用乙酸乙酯反萃取其中的待测物;乙酸乙酯中提取相经键合有磺酸基团的固相萃取柱浓缩、净化,待测物用氨化甲醇洗脱,洗脱液吹干,乙酸乙酯溶解定容;样品处理液分别用DB-1和DB-35色谱柱进行分离测定。结果方法在气相色谱火焰离子化检测器上的检出限为0.02 mg/kg,不同样品间加标回收率为85%~100%,RSD〈5.5%。结论本方法有效解决普通气相色谱在鉴定罂粟壳检测中灵敏度有限和定性能力弱的问题,可应用于基层实验室开展火锅底料等食品中违法添加罂粟壳的初筛检测。Objective To develop a method for the determination of papaverine in hotpot seasoning by double column- gas chromtography coupled with solid- phase extraction. Methods The papaverine were extracted out with HCl after the removal of oil from sample with hexane,and then to remove grease by removing the n- hexane; HCl extract was adjusted to alkaline with sodium hydroxide,and then ethyl acetate was used to back- extract the object to be measured; solid extraction column was used for concentration and purification,and the object to be measured was eluted with methanol ammoniation,dried,dissolved with ethyl acetate; sample treating liquid were separated and determined by using DB- 1 and DB- 35 chromatographic column. Results The results showed that the detection limit of the method was 0. 02 mg / kg,the recoveries rates of different samples were among 85%- 100%,and the relative standard deviations（ RSD） were less than 5. 5%. Conclusion This method can solve the problem of limited sensitivity and week identification capacity of common gas chromatography in the detection of papaveris,which can be widely applied in the prescreening of detecting papaveris in hotpot seasoning in the basic laboratories.

关 键 词：火锅底料 罂粟碱 双色谱柱分离 固相萃取 气相色谱法 

分 类 号：O657.71[理学—分析化学]