固相萃取/HPLC-MS/MS检测食品中吗啡等五种罂粟壳生物碱残留  

Determination of morphine and other four pericarpium papaveris alkaloid residues in hot pot seasonings and snack foods by solid phase extraction and HPLC-MS /MS

作　　者：张林田[1] 黄少玉 陆奕娜[1] 张冬辉[1] 杨晞[1] 孙锋伟 

机构地区：[1]汕头出入境检验检疫局,汕头515041 [2]汕头市疾病预防与控制中心,汕头515031

出　　处：《分析试验室》2014年第6期722-725,共4页Chinese Journal of Analysis Laboratory

基　　金：汕头市2011年科技项目(汕市财教[2011]134-116)资助

摘　　要：建立了同时检测食品中非法添加罂粟壳所产生的吗啡、可待因、蒂巴因、那可汀、罂粟碱残留量的固相萃取/HPLC-MS/MS方法。样品用体积分数1%三氯乙酸与乙腈混合液提取、正已烷脱脂后的净化液直接用PCX固相萃取柱净化。以乙腈-10 mmol/L乙酸铵为流动相、梯度洗脱、CR色谱柱分离、液相色谱-串联质谱联用仪检测,ESI（＋）SRM模式、标准曲线外标法检测吗啡等5种生物碱。化合物标准曲线相关系数均≥0.996,定量限均为0.5,1.0,5.0μg/kg,3个浓度添加水平的回收率在62.2%～117.9%之间,相对标准偏差在5.1%～17%（n=6）之间。Abstract： A method for simultaneous detection of morphine, codeine, thebaine, narcotine and papaverine residues which produced by illegal addition of pericarpium papaveris in hot pot seasonings and snack foods by solid phase extraction and HPLC -MS/MS was established . The sample was extracted by mixture of 1%trichloroacetic and acetonitrile, degreased with N -hexane and the purged liquid was purified directly by a PCX solid - phase extraction column. With acetonitrile - 10 mmol/L of ammonium acetate as mobile phase, the liquid was gradiently eluted and separated by a CR chromatographic column. Morphine and the other four alkaloids were determined by HPLC - MS/MS in ESI （ ＋ ） SRM mode with the external standard quantitation method. The correlation coefficients of standard curves for five alkaloids were ≥0.996. The quantitative detection limits of five alkaloids were 0.5μg/kg. The recoveries at three concentration levels of 0.5,1.0 and 5.0 μg/kg were between 62.2% and 117.9%. The relative standard deviations were between 5.1% and 17% （n = 6）. This method has the characteristics of simpleness, rapidness, high sensitivity and selectivity, qualitative reliability and quantitative accuracy etc.

关 键 词：HPLC-MS MS 罂粟壳 吗啡 可待因 罂粟碱 

分 类 号：O657.63[理学—分析化学]