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气相色谱-质谱法测定五粒回春丸中6种挥发性成分含量

Determination of Six Volatile Compounds in Wuli Huichun Pills by Gas Chromatogra-phy-Mass Spectrometry Method
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摘要 目的建立气相色谱-质谱(GC-MS)法同时测定五粒回春丸中挥发性成分麝香酮、薄荷脑、龙脑、异龙脑、樟脑、香芹酮的含量,对五粒回春丸进行质量评价。方法五粒回春丸乙酸乙酯提取液的分析采用HP-5MS毛细管柱(30 m×0.25 mm,0.25μm),进样口温度230℃,分流比10:1,载气为高纯氦气,进样口为恒流模式,载气流速为1.0 mL·min^(-1),程序升温。以三重四级杆串联质谱仪检测,离子源为电子轰击源(EI),离子源温度250℃。碰撞气为氩气。质谱传输接口温度250℃。扫描方式为SIM模式,溶剂延迟2.0 min。结果6种成分在各自范围内线性关系良好(r>0.9990),平均加样回收率93.57%~97.96%,相对标准偏差(RSD)0.73%~2.5%。结论该方法简便、准确、高效,可用于五粒回春丸的质量评价。 Objective To establish a gas chromatography-mass spectrometry method for simultaneous determination of the contents of volatile components muscone,menthol,borneol,isoborneol,camphor,and carvone in Wuli Huichun pills,and to evaluate the quality of Wuli Huichun pills based on authenticity,effectiveness and safety.Methods The ethyl acetate extract was analyzed by HP-5MS capillary column(30 m×0.25 mm,0.25μm)with temperature programming.The injection port temperature was set at 230℃,and the split ratio was set at 10:1.The carrier gas was high-purity helium gas.The injection port was in constant flow mode,with a carrier gas flow rate of 1.0 mL·min^(-1).The detector was a mass spectrometer with a triple quadrupole in series.The ion source was an electron bombardment source(EI)with a temperature of 250℃.The collision gas was argon.The temperature of the mass spectrometry transmission interface was 250℃.Scanning mode was SIM mode,with a solvent delay of 2 minutes.Results The linear relationships of the six components were good(r>0.9990),the average recoveries were 93.57%-97.96%,and the RSD was 0.73%-2.5%.Conclusion The method is simple,accurate,and efficient,and can be used for the quality evaluation of Wuli Huichun pills.
作者 李珊 李海燕 刘亚楠 王海波 茹庆国 黄霞 蒋芦荻 LI Shan;LI Haiyan;LIU Yanan;WANG Haibo;RU Qingguo;HUANG Xia;JIANG Ludi(Henan Institute for Drug and Medical Device Inspection,NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine(Chinese Materia Medica and Prepared Slices),Henan Province Engineering Research Center for Quality Control of Traditional Chinese Medicine,Zhengzhou 450018,China)
出处 《医药导报》 北大核心 2025年第9期1418-1422,共5页 Herald of Medicine
基金 2024年国家药品抽检计划(国药监药管[2024]1号)。
关键词 五粒回春丸 挥发性成分 气相色谱-质谱法 Wuli Huichun pills Volatile components Gas chromatography-mass spectrometry method
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