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作 者:高萌 丁锐 杨静 孔丽娟 齐喜红 GAO Meng;DING Rui;YANG Jing;KONG Lijuan;QI Xihong(Ningxia Hui Autonomous Region Institute of Drug Control,Ningxia Key Laboratory of Drug Creation and Generic Drug Research,Yinchuan 750004,China;Ningxia Mingde Healthy Pharmaceutical Corporation,Guyuan 756000,China)
机构地区:[1]宁夏回族自治区药品检验研究院,宁夏药物创新与仿制药研究重点实验室,银川750004 [2]宁夏明德中药饮片有限公司,固原756000
出 处:《宁夏医科大学学报》2024年第2期190-193,共4页Journal of Ningxia Medical University
基 金:宁夏药物创制与仿制药研究重点实验室开放课题(2018年)。
摘 要:目的建立超高效液相色谱-三重四极杆串联质谱(UPLC-MS/MS)法同时测定金莲清热胶囊中荭草苷、芒果苷、牡荆苷、毛蕊花糖苷和金丝桃苷的含量测定方法。方法采用Thermo Hypersil GOLD C18色谱柱(100 mm×2.1 mm,1.9μm),以0.1%甲酸水-乙腈为流动相,梯度洗脱,柱温35℃,流速0.2 mL·min^(-1)。电离方式为喷雾负离子模式(ESI-),多反应监测模式(MRM)用于定量分析。结果金莲清热胶囊中荭草苷等5种成分在考察浓度范围内呈现良好的线性关系(r>0.998);平均回收率(n=6)为98.3%~101.8%,RSD值为1.1%~1.8%。结论建立方法操作简便、准确度高、专属性强,可有效控制金莲清热胶囊的质量。Objective To establish a method for simultaneous determination of orientin,mangiferin,vitexin,verbascoside and hypericin in Jinlianqingre capsules by UPLC-MS/MS.Methods The separations were obtained on a Thermo Hypersil GOLD C18(100 mm×2.1 mm,1.9μm)with a gradient elution using the mixture of acetonitrile and 0.1%formic acid water solution as mobile phase.The flow rate was 0.2 mL·min^(-1),and the column temperature was set at 35℃.The multiple-reaction monitoring(MRM)scanning was employed for the quantification with switching electrospray ion source polarity in negative mode(ESI-).Results All calibration curves of 5 components were linear(r>0.998)over the tested ranges.The recoveries(n=6)ranged from 98.3%to 101.8%,and the RSD ranged from 1.1%to 1.8%.Conclusion The method is easy to operate,with high accuracy and strong specificity,which can be used for the quality control of Jinlianqingre capsules.
关 键 词:金莲清热胶囊 超高效液相色谱-三重四极杆串联质谱法 荭草苷 芒果苷 牡荆苷
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