滇紫草中肝毒性吡咯里西啶生物碱的含量分析  

Content Analysis of Hepatotoxic Pyrrolizidine Alkaloids in Onosmae Radicis Suber

作　　者：昝珂[1] 金红宇[1] 于健东[1] 杨铭 赵磊[3] ZAN Ke;JIN Hong-yu;YU Jian-dong;YANG Ming;ZHAO Lei(National Institutes for Food and Drug Control,Beijing 102629,China;Jining Research Institute for Food and Drug Inspection and Testing,Shandong Jining 272100,China;Siping Institute food and Drug Control,Jilin Siping 136000,China)

机构地区：[1]中国食品药品检定研究院,北京102629 [2]济宁市食品药品检验检测研究院,山东济宁272100 [3]四平市食品药品检验所,吉林四平136000

出　　处：《中国药物评价》2024年第5期368-371,共4页Chinese Journal of Drug Evaluation

基　　金：中国食品药品检定研究院关键技术研究基金(GJJS-2022-7-1)。

摘　　要：目的:建立液质联用法分析滇紫草中印美定、石松胺、蓝蓟定及其氮氧化物的含量。方法:采用沃特世HSS T3(长度100 mm、直径2.1 mm,粒径1.8μm)为色谱柱,以各含0.05%甲酸的乙腈水系统为流动相,梯度洗脱,流速为0.3 mL·min^(-1);进样量为1μL;电喷雾离子源,正离子多反应监测模式测定。结果:滇紫草中4种成分分别在0.972~97.2 ng·mL^(-1)、0.988~98.8 ng·mL^(-1)、1.024~102.4 ng·mL^(-1)、0.996~99.6 ng·mL^(-1)范围内线性关系良好(r>0.9990),回收率分别为93.5%、89.2%、88.1%和85.4%,RSD分别为3.5%、4.2%、3.2%和4.3%。结论:该方法专属性强,准确性好,可用于滇紫草中吡咯里西啶生物碱类成分的检测。Objective:To establish a UPLC-MS/MS method for the analysis of intermedine,lycopsamine,echimidine and echimidine N-oxide in Onosmae Radicis Suber.Methods:Four analytes were separatied by a HSS T3 column(length 100 mm,diameter 2.1 mm,particle size 1.8μm)with a mobile phase of acetonitrile-water(containing 0.05%formic acid,respectively)by gradient elution with the flow rate of 0.3 mL·min^(-1).The injection volume is 1μL.The MS system was operated by using electrospray ionization in the positive ion mode,and the scan mode was in multiple reactions monitoring mode.Results:The above-mentioned four components showed good linear relationships within the ranges of 0.972-97.2 ng·mL^(-1),0.988-98.8 ng·mL^(-1),1.024-102.4 ng·mL^(-1),and 0.996-99.6 ng·mL^(-1)(r>0.9990).The average recoveries were 93.5%,89.2%,88.1%,and 85.4%with RSD of 3.5%,4.2%,3.2%,and 4.3%,respectively.Conclusion:This method has strong specificity and good accuracy,and can be used for the detection of pyrrolizidine alkaloids in Onosmae Radicis Suber.

关 键 词：滇紫草 液质联用法 吡咯里西啶生物碱 含量测定 

分 类 号：R284.1[医药卫生—中药学]