摘要
目的:建立同时测定菟丝子中6种黄酮类化合物成分含量的高效快速的超高效液相色谱-串联质谱法(UPLC-MS/MS)方法。方法:采用Waters UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7μm),甲醇-0.1%甲酸水溶液为流动相,梯度洗脱,流速为0.3 ml/min,柱温为30℃;质谱条件采用ESI-离子源,多反应离子检测模式(multiple reaction monitoring,MRM),对菟丝子中6种黄酮类成分金丝桃苷、紫云英苷、异槲皮苷、槲皮苷、山萘酚、槲皮素进行含量测定。结果:在上述条件下测得各化合物分别在5.0~500 ng/ml线性范围内呈良好线性关系(r>0.999);精密度、重复性、回收率、稳定性均满足方法学验证要求。结论:该方法高效、准确、灵敏,可用于同时测定菟丝子中金丝桃苷、紫云英苷、异槲皮苷、槲皮苷、山萘酚、槲皮素的含量。
Objective:To develop a UPLC-MS/MS method for simultaneous determination of six flavonoids in Semen Cuscutae.Methods:The separation of the six flavonoids was performed on an ACQUITY UPLC BEH C18 column(50 mm×2.1 mm,1.7μm)at 30℃.The mobile phase consisted of methanol and aqueous 0.1%formic acid using gradient elution,which was delivered at a flow rate of 0.3 ml/min.The determination of the Hyperoside,Astragalin,Isoquercitrin,Quercitrin,Quercetin,and Kaempferol from Semen Cuscutae was performed on UPLC-MS/MS system with turbo ion spray source in the negative ion and multiple reactionmonitoring mode.Results:The method was linear over the concentration range of 5.0-500 ng/ml for the six analytes.All calibration curves showed good linearity(r>0.999).The precision,repeatability,recoveries were all conformed to the validated requirements of methodology.Conclusion:The developed and validated methods are efficient,accurate and selective for the separation and quantification of the six flavonoids in Semen Cuscutae.
作者
张威
付之恬
刘宸光
王博伦
刘润东
范荣华
ZHANG Wei;FU Zhitian;LIU CHENguang;WANG Bolun;LIU Rundong;FAN Ronghua(Grade 2015,Shenyang Medical College,Shenyang 11034,China;Grade 2017,Shenyang Medical College;Grade 2014 Shenyang Medical College;Department of Health Inspection Shenyang Medical College)
出处
《沈阳医学院学报》
2018年第4期377-380,共4页
Journal of Shenyang Medical College
基金
沈阳医学院科技基金项目(No.20163042)
沈阳医学院大学生科研立项(No.20179034)
沈阳市科技计划项目(No.17-231-1-45)