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作 者:王芝燕 刘辉[1] 李均艳 刘永利 孙慧珠 WANG Zhiyan;LIU Hui;LI Junyan;LIU Yongli;SUN Huizhu(Department of Pharmacy,Wujin Traditional Chinese Medicine Hospital of Changzhou City,Changzhou 213161,China;Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050227,China)
机构地区:[1]常州市武进中医医院药剂科,常州213161 [2]河北省药品医疗器械检验研究院,石家庄050227
出 处:《医药导报》2022年第8期1193-1198,共6页Herald of Medicine
摘 要:目的采用液相色谱-三重四级杆质谱(UPLC/MS/MS)含量测定法,同时测定咳喘合剂中盐酸麻黄碱、盐酸伪麻黄碱、阿魏酸、苦杏仁苷、贝母素甲、贝母素乙、甘草苷、甘草次酸8种特征成分的含量,实现快速定性定量分析。方法样品经70%乙醇超声处理后,采用C18(2.1 mm×100 mm,2.6μm)色谱柱,以甲醇-0.1%甲酸为流动相进行梯度洗脱,流速0.3 mL·min-1;电喷雾正负离子源同时监测,多反应监测(MRM)模式。通过比较样品与对照品的色谱保留时间、离子对、色谱峰面积,同时对8种成分进行定量测定。结果方法重复性准确度良好,平均回收率在101.1%~106.6%范围内,RSD为2.2%~4.1%,样品测定结果表明制剂批次间一致性良好。结论该方法快速简便,选择性好,准确可靠,为咳喘合剂的质量控制提供科学依据。Objective To simultaneously determine the contents of Kechuan Mistura,like ephedrine hydrochloride,pseudoephedrine hydrochloride,ferulic acid,amygdalin,peimine,peiminine,liquiritin and glycyrrhetinic acid to achieve rapid qualitative and quantitative analysis.Methods The sample was ultrasonicated with 70%ethanol.The chromalographic separation was proformed on a C18 column(2.1 mm×100 mm,2.6μm)with methanol-0.1%formic acid solution as mobile phases in a gradient elution.The flow rate was 0.3 mL·min-1.The analytes were detected by tandem mass spectrometry under the positive and negative ion mode with the ESI source and carried out in the multiple reaction monitoring(MRM)mode.Results The repeatability and accuracy of the method were good,and the average recovery rate was 101.1%—106.6%,and RSDs were 2.2%—4.1%.The sample determination results showed good batch-to-batch consistency.Conclusion The developed method in the study is simple,rapid,specific,accurate and reliable.It provides a more comprehensive scientific basis for the quality evaluation of Kechuan Mistura.
关 键 词:咳喘合剂 含量测定 液相色谱-三重四级杆质谱 多反应监测 质量控制
分 类 号:R917[医药卫生—药物分析学]
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