应用液质联用法(LC-MS/MS)快速测定药酒中11种钩吻生物碱的含量  

Rapid determination of the levels of 11 gelsemium alkaloids in medicinal liquor by liquid chromatography with tandem mass spectrometry(LC-MS/MS)

作　　者：陈杰[1] 钟延旭[1] 雷宁生[1] CHEN Jie;ZHONG Yanxu;LEI Ningsheng(Guangxi Zhuang Autonomous Region Center for Disease Control and Prevention,Nanning,Guangxi 530028,China)

机构地区：[1]广西壮族自治区疾病预防控制中心,广西南宁530028

出　　处：《应用预防医学》2023年第5期321-324,329,共5页Applied Preventive Medicine

基　　金：广西壮族自治区卫生和计划生育委员会自筹经费科研课题(2015455)。

摘　　要：目的建立高效液相色谱-质谱联用法(液质联用法,LC-MS/MS)测定药酒中钩吻素甲等11种钩吻生物碱的含量,以期为药酒中毒事件中样品的钩吻碱等生物碱的应急检测提供参考。方法采用LC-MS/MS法,色谱柱为Agilent ZORBAX Eclipse XDB C18柱(2.1×150 mm,3.5μm);柱温为40℃;流动相中A相为0.1%甲酸水溶液,B相为0.1%甲酸乙腈;流速为0.5 mL/min;以钩吻素甲等11种钩吻生物碱为标准对照品,同时测定药酒样品中各物质含量。结果11种钩吻生物碱在5.0~300.0 ng/mL范围内线性关系良好,相关系数为0.9981~0.9998,回收率在85.2%~98.4%之间,检出限为0.1~0.6μg/kg,定量限为0.3~2.0μg/kg。结论高效液相色谱-质谱联用法具有选择性强、灵敏度好、准确度高的优势,可用于药酒样品中生物碱的快速定性和定量。Objective To establish a high-performance liquid chromatography-mass spectrometry tandem method(liquid chromatography with tandem mass spectrometry, LC-MS/MS) for the determination of 11types of gelsemine in medicinal liquor, providing a reference for the emergency detection of gelsemine and other alkaloids in samples during medicinal liquor poisoning incidents. Methods LC-MS/MS method was used. The chromatographic column was Agilent ZORBAX Eclipse XDB C18 column(2.1×150 mm,3.5 μm);the column temperature was 40°C;phase A in the mobile phase was 0.1% formic acid aqueous solution, and phase B was 0.1% formic acid, with a flow rate of 0.5 mL/min. Using 11 types of gelsemine as the standard reference substances, and the content of each substance in the medicinal liquor samples was determined simultaneously.Results The linear relationship of 11 types of gelsemine was superior within the range of 5.0-300 ng/mL,with a correlation coefficient of 0.9981-0.9998, a recovery rate of 85.2%-98.4%, a detection limit of 0.1-0.6μg/kg, and a quantitative limit of 0.3-2.0 μg/kg.Conclusions High-performance liquid chromatography-mass spectrometry tandem method has the advantages of strong selectivity, high sensitivity, and high accuracy to be used in rapid identification and quantification of alkaloids in medicinal liquor samples.

关 键 词：高效液相色谱-质谱联用法 药酒 钩吻碱 11种生物碱 

分 类 号：R155.5[医药卫生—营养与食品卫生学]