【作者】 张启云； 徐国良； 黄丽萍； 马晓雪； 曾治君； 余日跃； 刘红宁；

【Author】 Qiyun Zhang~1 Guoliang Xu~1 Liping Huang~2 Xiaoxue Ma~1 Zhijun Zeng~2 Riyue Yu~2 Hongning Liu~2 1.Key laboratory of Modem Preparation(Jiangxi University of Traditional Chinese Medicine),Ministry of Education,Nanchang Jiangxi 330004; 2.Jiangxi University of TCM,Nanchang Jiangxi 330006

【机构】 江西中医学院现代中药制剂教育部重点实验室； 江西中医学院；

【摘要】 目的:建立一种快速测定大鼠尿液中吴茱萸碱和吴茱萸次碱的定量方法。方法:用三重四级杆串联质谱(MS’MS) 作为 HPLC 的检测器,其中 MS/MS 使用了多反应检测(MRM)扫描方式。分别选择304.2→134.2和288.2→244.2离子对 m/z 作为 MRM 检测的离子对;流动相:甲醇:水(85:15)内含5mM 甲酸铵;色谱柱:Agilent Zorbax XDB-C18,以测定大鼠尿液中吴茱萸碱和吴茱萸次碱为例,对此方法进行了应用。结果:方法的线性范围为吴茱萸碱:5.615-1437.5ng/ml(γ=0.999), 检测限1.87ng/ml,吴茱萸次碱:10.26-1314.25ng/ml(γ=0.998),检测限5.13ng/ml。结论:此法灵敏、准确,可用于含茱萸碱和吴茱萸次碱的药物代谢研究。更多还原

【Abstract】 Objective:To establish a method for quantitative analysis of evodiamine and rutaecarpine in rat urine rapidly.Method:A triple-quadrupole tandem mass spectrometry was used as the detector of HPLC.As to MS/MS,multi-reactions monitoring(MRM) scan mode was employed.Among the product ions of evodiamine and rutaecarpine,m/z-134.2 and 244..2 are the most abundant in intersity, thus the parent-daughter ion pairs of m/z 304.2→134.2 and 288.2→244.2 were selected as MRM ions pairs.MS/MS conditions were optimized to achieve highest sensitivity.The mobile phase of HPLC was methanol-water (85:15) containing 5mM ammonium formate. The analytical column was Agilent Zorbax XDB-C 18.The flow rate of HPLC was 0.5ml/min.The areas of ion flow peaks were used to determine the content of evodiamine and rutaecarpine in the rat urine.Result:The standard curves for evodiamine and rutaecaroine showed good linearity over ranges of 5.615-1437.5ng/ml(γ=0.999) and 10.26-1314.25ng/ml(γ=0.998),and the detection limit for evodiamine and rutaecarpine were 1.87ng/ml and 5.13ng/ml respectively.Conclusion:This method is highly sensitive,fast and very accurate.Therefore,it is possible to be applied to study the metabolism of evodiamine and rutaecarpine.更多还原