液质联用法测定止咳类中成药中5种罂粟壳生物碱  

Detection of 5 alkaloids in papaveris in antitussive traditional Chinese medicine with liquid chromatography mass spectrometry

作　　者：刘敏敏[1] 刘利颜[1] 刘丛丛[1] LIU Min - min LIU Li -yan LIU Cong - cong(Guangdong Institute for Drug Control, Guangzhou, Guangdong 510180, China)

机构地区：[1]广东省药品检验所,广东广州510180

出　　处：《中国卫生检验杂志》2016年第23期3353-3356,共4页Chinese Journal of Health Laboratory Technology

基　　金：广东省中医药局"建设中医药强省科研课题"(2014-2027)

摘　　要：目的建立止咳类中成药中非法添加的罂粟壳中吗啡、可待因、罂粟碱、那可丁、蒂巴因共5种生物碱的液质联用测定方法。方法用稀盐酸提取罂粟壳中的生物碱,用Kinetex HILIC色谱柱(2.1 mm×100 mm,2.6μm)进行分离,0.1%甲酸的乙腈溶液-0.1%甲酸的10 mmol/L甲酸铵溶液为流动相梯度洗脱,流速为0.3 ml/min。结果吗啡、可待因线性范围为50 ng/ml^250 ng/ml,罂粟碱、蒂巴因和那可丁线性范围为1 ng/ml^50 ng/ml。吗啡的检出限为38μg/kg,可待因的检出限为27μg/kg,罂粟碱、蒂巴因和那可丁的检出限为8μg/kg,加标回收率为71.4%~102.8%。对39批次止咳中成药进行测定,其中2批检测结果为阳性,含量分别为一批吗啡含量为253.4μg/kg,可待因含量为35.5μg/kg,另一批吗啡含量为442.0μg/kg,可待因含量为54.1μg/kg。结论本方法适用于止咳类中成药中5种罂粟壳生物碱的测定。Objective To establish a liquid chromatography mass spectrometry（ LC-MS/MS） method for the determination of morphine,codeine,narceine,narcotine,thebaine added in antitussive traditional Chinese medicine. Methods Alkaloids residues in papaveris were extracted by dilute hydrochloric acid. Chromatographic separation was carried out on a Kinetex HILIC column（ 2. 1 mm × 100 mm,2. 6 μm）,and the alkaloids residues were gradient eluted with the mobile phase,the constitute of which was acetonitrile solution containing 0. 1% formic acid and 10 mmol/L ammonium formate solution containing 0. 1% formic acid. The flow rate was 0. 3 ml/min. Results The linear relationship was good in the range of 50 ng/ml-250 ng/ml for morphine and codeine,1 ng/ml-50 ng/ml for narceine,thebaine and narcotine. The detection limit of morphine was 38 μg/kg,that of codeine was 27 μg/kg,and the others were 8 μg/kg. The recovery of standard addition was within 71. 4%-102. 8%.39 batches of anti-cough traditional Chinese medicine were determined,in which 2 batch of test results were positive. The contents of morphine and codeine in one batch were 253. 4 μg/kg and 35. 5 μg/kg; and that in the other batch were 442. 0 μg/kg and 54. 1 μg/kg. Conclusion The method is suitable to the detection of the 5 alkaloids in papaveris illegally added in antitussive traditional Chinese medicine.

关 键 词：罂粟壳 生物碱 止咳类中成药 液质联用法 

分 类 号：O657.63[理学—分析化学]