【摘要】 目的建立麻辣烫及汤料中罂粟壳中罂粟碱、吗啡、那可丁、可待因和蒂巴因的超高效液相色谱-串联质谱检测方法。方法样品用稀盐酸加热超声提取,正己烷除脂,阳离子固相萃取柱净化,5%氨化甲醇洗脱,用超高效液相色谱-串联质谱(UPLC-MS/MS)检测。HSS T3柱分离,以0.1%甲酸-10 mmol/L甲酸铵水溶液-0.1%甲酸乙腈溶液作为流动相进行梯度洗脱,正离子多反应监测模式检测。目标药物使用基质外标法定量。结果 5种目标药物的线性范围为0.1μg/L~500μg/L,相关系数均>0.99。方法定量检出限为0.1μg/kg~1.25μg/kg,3个加标水平下的回收率为64.0%~120%,相对标准偏差为1.2%~11%。结论本方法操作简单、测定结果准确,可用于麻辣烫和汤料中罂粟壳生物碱成分的测定。更多还原

【Abstract】 Objective To establish a method for the detection of 5 poppy husk alkaloids( papaverine,noscapine,morphine,codeine and thebaine) in Malatang and its seasoning by ultra high performance liquid chromatography-tandem mass spectrometry( UHPLC-MS/MS). Methods The samples were ultrasonically extracted with dilute Hcl solution under heating condition.Lipid in the sample solution was removed with hexane. Purification was carried out on a mixed-cation solid-phase extraction column( MCX) and 5% aqueous ammonia with methanol was used for elution,and finally the target alkaloids were separated and detected by UHPLC-MS/MS. The separation was performed on an HSS T3 column with a mobile phase of acetonitrile-10 mmol/L ammonium acetate-0. 1% formic acid by gradient elution. A multiple reaction monitoring( MRM) mode was employed in mass spectrometric detection. The matrix-matched external standard calibration was used for the quantification.Results Good linearities of the method were obtained when the concentration was within 0. 1 μg/L-500 μg/L,with the correlation coefficients( r) above 0. 99. The method quantitation limits( MQL) were in the range of 0. 1μg/kg-1. 25 μg/kg. Average recoveries at three spiked levels ranged from 64. 0% to 120%,with relative standard deviations( RSDs) of 1. 2%-11%.Conclusion This method is simple,accurate and sensitive. It can be used for the detection of 5 alkaloids in opium poppy husk in Malatang and its seasoning.更多还原