本研究采用超高液相色谱-串联质谱技术，建立了同时测定粮谷中双氢麦角汀、麦角柯宁碱、麦角异柯宁碱、麦角克碱、麦角异克碱、麦角卡里碱、麦角异卡里碱、麦角生碱、麦角胺等9种麦角生物碱的方法。样品采用乙腈-水溶液（84+16）提取，经分散固相萃取剂PSA净化后，超高液相色谱-串联质谱仪测定，C18柱分离，以0.1%甲酸水溶液和乙腈为流动相梯度洗脱，外标法定量。麦角碱检出限均为5 μg/kg，定量限均为20 μg/kg，在45~375 μg/kg添加浓度下，麦角碱的回收率为50%~90%。同时通过高分辨质谱，确定麦角碱的一级精确质量数以及二级特征碎片离子，辅助样本筛查确证。对20份市售粮谷样品进行检测，有一份样本检出了麦角克碱和麦角异克碱，其含量高于检出限而低于定量限。本研究为粮谷及其制品中麦角碱提供相对有效的检测方法，保障我国粮谷安全。

In this study, ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was used to establish a method for simultaneous determination of nine ergot alkaloids in cereals including dihydroergocristine, ergocornine, ergocorninine, ergocristine, ergocristinine, ergocryptine, ergocryptinine, ergosine, and ergotamine. The sample was extracted with an acetonitrile-water (84+16) solution, and the extract was purified with dispersive solid phase extraction agent (PSA). The UPLC-MS/MS analysis employed a C18 column for separation, and a mobile phase consisting of 0.1% formic acid aqueous solution and acetonitrile for gradient elution, along with external standards for quantification. The limit of detection (LOD) and limit of quantitation (LOQ) of ergot alkaloids were 5 μg/kg and 20 μg/kg, respectively. The recovery of ergot alkaloids was in the range of 50%~90% at the concentration of 45~75 μg/kg. At the same time, high-resolution mass spectrometry (HRMS) was used to determine the accurate mass and the secondary characteristic fragment ions of ergot alkaloids, to assist sample screening and confirmation. Twenty commercially available cereal samples were tested, with ergocristine and ergocristinine were detected in one sample and its content higher than the LOD but lower than the LOQ. This study provides a relatively effective detection method for ergot alkaloids in cereals and their products to ensure the safety of grains in China.

国家重点研发计划项目（2018YFC1602302）；湖北省食药局重点科研项目（201802002）