固相萃取-液质联用测定火锅底料中5种生物碱

Determining of Five Alkaloids Residues in Hotpot Seasoning Using Solid-phase Extraction-high Performance Liquid Chromatography-tandem Mass Spectrometry

建立双柱串联固相萃取-高效液相色谱-串联质谱法（HPLC-MS/MS）测定火锅底料中罂粟碱、吗啡、那可丁、可待因和蒂巴因5种生物碱成分的含量。样品用酸化乙腈提取,PSA和PXC固相萃取柱串联净化,经Hillic色谱柱分离,以电喷雾离子源（ESI）在正离子多反应监测（MRM）模式下进行测定,内标法定量。在优化的试验条件下,罂粟碱、吗啡、那可丁、可待因、蒂巴因的检出限分别为0.033、1.5、0.066、1.2、0.15μg/kg。5种生物碱类药物在3个加标水平下的回收率范围为96.0%～112.5%,RSD为2.0%～5.7%。该方法操作简便、准确、灵敏度高,适用于火锅底料中罂粟碱、吗啡、那可丁、

A method was developed for the determination of five alkaloids residues in hotpot seasoning by dual solid-phase extraction clean up-high performance liquid chromatography-tandem mass spectrometry（HPLCMS/MS）. The residues were extracted from the samples by acetonitrile,cleaned up with PSA and PXC solid phase extraction cartridges,then analyzed by using HPLC-MS/MS in multiple reaction monitoring（MRM）mode via positive electrospray ionization with an Hillic column as the analytical column. An internal standard method was used for quantitative determination of five alkaloids. The limits of determination for papaverine,morphine,noscapine,codeine and thebaine were 0.033,1.5,0.066,1.2,0.15 μg/kg,respectively. The recoveries for the five alkaloids,at three fortified levels,ranged from 96.0 % to 112.5 %,with relative standard deviations between 2.0 % and 5.7 %.The method was simple,accurate and sensitive. It was suitable for the determination of alkaloids residues in hotpot seasoning.