72种生物碱高分辨质谱数据库建立与应用  

Establishment and application of 72 alkaloids database with high resolution mass spectrometry

作　　者：唐晓琴[1] 赵舰[1] 贺丽迎 甘源[1] 周春艳[1] 程莉[1] 覃梅[1] TANG Xiaoqin;ZHAO Jian;HE Liying;GAN Yuan;ZHOU Chunyan;CHENG Li;QIN Mei(Chongqing Center for Disease Control and Prevention,Chongqing 400042,China)

机构地区：[1]重庆市疾病预防控制中心,重庆400042

出　　处：《中国食品卫生杂志》2020年第3期228-233,共6页Chinese Journal of Food Hygiene

基　　金：重庆市卫生健康委员会重点课题:运用高分辨质谱技术建立常见生物碱数据库及生物碱中毒检测方法研究(2017ZDXM002)。

摘　　要：目的建立常见生物碱的高分辨质谱数据库并应用于中毒样品的自动筛查。方法将生物碱标准品溶液以流动注射方式直接导入四极杆/静电场轨道阱高分辨质谱仪,或经高效液相色谱分离后进行质谱分析,得到准分子离子峰的精确质量数和合适的碰撞能量,采用HSS T3色谱柱(2.1 mm×100 mm,1.8μm),以甲醇和5 mmol/L乙酸铵-0.1%甲酸水溶液为流动相,梯度洗脱,电喷雾电离源正离子模式(HESI^+)和tSIM-ddMS^2模式下分析,采集生物碱的二级质谱信息,并将此质谱数据用于实际样品的自动筛查。结果获得了72种生物碱的精确分子量、保留时间、碰撞能量、碎片离子等信息并建立了质谱库,通过Full mass模式进样,仪器自动检索可快速锁定实际样品中含有的多种生物碱。结论该方法操作简便、灵敏度高,可满足中毒样品中生物碱快速自动筛查的要求。Objective The high resolution mass spectra database of common alkaloids were established and applied to the automatic screening of poisoning samples.Methods The accurate molecular mass and appropriate collision energy of each alkaloid was obtained by injecting alkaloid standard solutions into the Q exactive mass spectrometry directly or separated by high performance liquid chromatography and mass spectrometry analysis.The chromatographic analysis was performed on a HSS T3 column(2.1 mm×100 mm,1.8μm)by gradient elution using methanol and 5 mmol/L ammonium acetate containing 0.1%formic acid solution as mobile phase.The secondary mass information of alkaloid was collected in positive electrospray ionization and targeted-selected ion monitor-ddMS^2 mode.The mass spectrometry data were applied to the automatic screening of actual samples.Results The mass spectrometry database of 72 alkaloids were established containing the theoretical accurate molecular mass,retention time collision energy and fragment ions.The multiple alkaloids in actual samples were locked rapidly by automatic screening with the mass spectra database.Conclusion This method is simple,fast,accurate and suitable for the rapid automatic screening of alkaloids in poisoned food sample.

关 键 词：高分辨质谱 生物碱 自动筛查 质谱数据库 

分 类 号：R155[医药卫生—营养与食品卫生学]