基于超高效液相色谱-串联质谱法研究大黄蒽醌苷元在大鼠体内的药代动力学  

Pharmacokinetics of Dahuang(Rhubarb)Anthraquinonesapogenins in Rats Based on Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：宋靖宇 管秀璐 马烨超 沈诗嫄 李云迪 刘翠哲[1] SONG Jingyu;GUAN Xiulu;MA Yechao;SHEN Shiyuan;LI Yundi;LIU Cuizhe(Chengde Medical College,Hebei Province Key Laboratory of Traditional Chinese Medicine Research and Development,Chengde Hebei 067000,China)

机构地区：[1]承德医学院/河北省中药研究与开发重点实验室,河北承德067000

出　　处：《中医药导报》2024年第5期41-49,共9页Guiding Journal of Traditional Chinese Medicine and Pharmacy

基　　金：河北省中央引导地方科技发展项目—科技创新基地项目(216Z2502G);河北省自然科学基金中医药联合基金资助项目(H2022406043);承德医学院学科建设经费(2023LJ-1);承德医学院高层次人才科研启动基金项目(202210)。

摘　　要：目的:建立超高效液相色谱-串联质谱(UPLC-MS/MS)法同时测定芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚在大鼠血浆中浓度的方法。方法采用AB SciexQtrap5500三重四极杆液质联用系统,色谱柱为Waters UPLC BEH C_(18)柱(100.0 mm×2.1mm,1.7μm),体积流量为0.3 mL/min,柱温为25.0℃,进样量为3μL,流动相为0.1%甲酸-乙腈梯度洗脱。采用电喷雾离子源,多反应监测模式进行检测。结果:芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚分别在1.000~64.000、1.000~1000.000、0.300~32.000、1.000~250.000和1.000~64.000μg/m L质量浓度范围内与峰面积呈良好的线性关系,标准曲线的相关系数均在0.99~1.00之间,大黄素的定量限为0.3μg/mL,其余4种大黄蒽醌成分定量限均为1.0μg/mL;精密度和稳定性试验的RSD值均小于8.7%;平均加样回收率为88.7%~98.8%,RSD值为0.9%~2.4%;基质效应在89.8%~96.2%之间。结论:本研究建立的UPLC-MS/MS法简单、快速、准确灵敏,可用于大黄蒽醌苷元在大鼠体内的含量测定。Objective:To establish a UPLC-MS/MS method for the simultaneous measurement of rat plasma concentrations of aloe-emodin,rhein,emodin,chrysophanol and physcion.Methods:The AB SciexQtrap5500 triple quadrupole LC/MS system was used for the Waters UPLC BEH C_(18) column(100.0 mm×2.1 mm,1.7μm),with a volume flow rate of 0.3 mL/min,a column temperature of 25.0℃,an injection volume of 3μL,and a mobile phase of 0.1%formic acid-acetonitrile gradient elute.The electron spray ionization was adopted,and the working mode was a multi-reaction monitoring mode.Results:Aloe-emodin,rhein,emodin,chrysophanol and physcion showed good linear relationships with peak areas in the concentration ranges of 1.000-64.000,1.000-1000.000,0.300-32.000,1.000-250.000 and 1.000-64.000μg/mL,respectively,with the correlation coefficients of the standard curves in the range of 0.99-1.00.The limits of quantification(LOQs)of emodin were 0.3μg/mL,and those of the other four rhubarb anthraquinones were 1.0μg/mL.The RSD of the precision and stability tests were less than 8.7%.The average recoveries of spiked standards ranged from 88.7%to 98.8%,with RSD of 0.9%-2.4%,and the matrix effects ranged from 89.8%to 96.2%.Conclusion:The UPLC-MS/MS approach developed in this study is straightforward,quick,precise,and sensitive,and it may be utilized to estimate the anthraquinonesa-pogenins concentration of Dahuang(rhubarb)in rats.

关 键 词：大黄蒽醌 药代动力学 超高效液相色谱-串联质谱法 含量测定 大鼠 

分 类 号：R285.5[医药卫生—中药学]