气相色谱-质谱法测定食品中罂粟壳提取物的残留量  

GC-MS Determination of Residual Poppy Shell Extract in Food

作　　者：沈平[1] 谢朝梅[1] 谢燕湘[1] 

机构地区：[1]常德市疾病预防控制中心,常德415000

出　　处：《理化检验（化学分册）》2016年第1期48-51,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：采用气相色谱-质谱法检测食品中罂粟壳提取物中的可待因、吗啡、蒂巴因、罂粟碱和乙基吗啡。样品中罂粟壳提取物在酸性溶液中水解溶出后,在中性溶液中用乙腈提取,脱水离心后取其上清液用N-丙基乙二胺、无水硫酸镁、C18的混合试剂净化,净化液用N,O-双三甲基硅基三氟乙酰胺-三甲基氯硅烷(99+1)衍生后,在Rxi-5ms色谱柱上分离,质谱分析中采用电子轰击离子源和选择离子监测模式。5种化合物在一定范围内呈线性,检出限(3s/k)在0.01~0.03 mg·L^(-1)之间。加标回收率在81.5%~96.4%之间,测定值的相对标准偏差(n=6)在1.6%~5.9%之间。GC-MS was applied to the determination of codeine, morphine, tibane, apaverine and ethyl morphine in poppy shell extract in food. Poppy shell extract in the sample was hydrolyzed and dissolved in an acidic solution, and then the solution was extracted with acetonitrile from neutral solution. After dehydration and centrifugation, the supernatant was purified with a mixed reagent of N-propylethylene diamine, anhydrous magnesium sulfate and C18. The purified solution was derivatized with the mixture of N, O-bis（trimethylsilyl） trifluoroacetamide and trimethylchlorosilane （99＋1）. The analytes were separated on an Rxi 5ms column. E1 and SIM were adopted in MS. Linear relationships were found between the peak areas and the mass concentration of 5 componds in definite ranges, with detection limits （3s/k） in the range of 0. 01-0. 03 mg. L- 1. Recovery rates obtained by standard addition method were in the range of 81.5%-96.4% and RSDs （n=6） were in the range of 1.6%-5.9%.

关 键 词：气相色谱-质谱法 罂粟壳 提取物 衍生 

分 类 号：O657.63[理学—分析化学]