基于《德国药品法典》要求的南五味子质量控制方法研究  

Quality Control Methods of Schisandrae Sphenantherae Fructus Based on Requirements of Deutscher Arzneimittel-Codex

作　　者：卢晨娜 向定华 许海玉[1] 王梅 孙朋悦 李皓月 冯伟红[1] 刘晓谦[1] 李春[1] 宋坪[4] LU Chen-na;XIANG Ding-hua;XU Hai-yu;WANG Mei;SUN Peng-yue;LI Hao-yue;FENG Wei-hong;LIU Xiao-Qian;LI Chun;SONG Ping(National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicine,Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China;Leiden University-European Center for Chinese Medicine and Natural Compound,Leiden 2333BE,The Netherlands;SU BioMedicine,Leiden 2333 BD,The Netherlands;China Academy of Chinese Medical Sciences,Beijing 100700,China)

机构地区：[1]中国中医科学院中药研究所,中药质量控制技术国家工程实验室,北京100700 [2]莱顿大学-欧洲天然产物与中医药研究所,莱顿2333BE [3]SU生物医药,莱顿2333BD [4]中国中医科学院,北京100700

出　　处：《中国现代中药》2024年第9期1494-1502,共9页Modern Chinese Medicine

基　　金：中国-荷兰中医药防治重大感染性疾病“一带一路”联合实验室建设项目(Z211100007921004)。

摘　　要：目的:依据《德国药品法典》(Deutscher Arzneimittel-Codex,DAC)的相关规定,建立符合DAC要求的南五味子薄层色谱鉴别方法和含量测定方法,并比较DAC与《中华人民共和国药典》(以下简称《中国药典》)2020年版对以上2项内容规定的异同点。方法:采用硅胶GF254薄层色谱板,以乙酸-乙酸乙酯-甲苯(1∶18∶46)为展开剂,以五味子乙素和五味子醇乙为系统适应性测试(SST)指标,以五味子酯甲和五味子甲素为检测指标建立了南五味子的薄层色谱鉴别方法。以HALO Biphenyl色谱柱(250 mm×4.6 mm,5μm)为固定相,乙腈-水为流动相进行梯度洗脱,检测波长为254 nm,流速为0.8 mL·min^(-1),柱温为35℃,以五味子酯甲和五味子酯乙的分离度为SST评价指标考察方法的可行性,建立了南五味子药材中五味子酯甲和五味子甲素的高效液相色谱法(HPLC)含量测定方法。结果:按照DAC相关要求进行了SST考察,结果显示,建立的薄层色谱鉴别方法具有良好的分离能力,可满足南五味子药材薄层色谱鉴别的要求;HPLC测定结果中五味子酯甲和五味子酯乙的分离度均大于3.5,符合SST要求,可用于南五味子含量测定;方法学考察结果均符合含量测定要求;31批五味子药材中五味子酯甲和五味子甲素的质量分数分别为0~0.7611%和0.0109%~0.7909%,且2个成分含量呈正相关。结论:建立的南五味子薄层色谱鉴别方法和HPLC含量测定方法均符合DAC要求,且操作简便、结果准确、重复性好,可用于南五味子的质量控制;在药材的薄层色谱鉴别及含量测定方法方面,DAC与《中国药典》2020年版大致相同,但在SST方面存在差异,应加以重视。Objective:To establish the methods for identifying Schisandrae Sphenantherae Fructus based on thinlayer chromatography(TLC)and determining the content of indicator components according to the relevant requirements of Deutscher Arzneimittel-Codex(DAC),and compare the requirements on the identification and content determination between DAC and Chinese Pharmacopoeia(2020 edition).Methods:The TLC-based identification method for Schisandrae Sphenantherae Fructus was established with silica gel GF254 thin-layer plate as the immobile phase,acetic acid-ethyl acetate-toluene(1:18:46)as the developing solvent,schizandrin B and gomisin A as indicators of system suitability test(SST),and schisantherin A and schizandrin A as detection indicators.The high performance liquid chromatography(HPLC)-based method for simultaneously determining the content of schisantherin A and schizandrin A was established with a HALO Biphenyl column(250 mm×4.6 mm,5μm)as the immobile phase and acetonitrile-water as the mobile phase for gradient elution at a flow rate of 0.8 mL·min-1 and a column temperature of 35℃.The resolution of schisantherins A and B was used as the indicator of SST to examine the feasibility of the established method.Results:We conducted SST in accordance with the requirements in DAC.The SST results showed that the TLC-based method had good separation ability and met the identification requirements of Schisandrae Sphenantherae Fructus.The resolution of schisandrins A and B in the established HPLC-based method was above 3.5,indicating that the method met the requirements of DAC on SST and can be used for determining the content of indicator components in Schisandrae Sphenantherae Fructus.The results of methodological investigations demonstrated that the established HPLC-based method met the requirements for content determination.The content of schisantherin A and schizandrin A in 31 batches of Schisandrae Sphenantherae Fructus samples varied within the ranges of 0-0.7611%and 0.0109%-0.7909%,respectively.Moreover,the conten

关 键 词：南五味子 《德国药品法典》 薄层色谱鉴别 含量测定 五味子酯甲 五味子甲素 

分 类 号：R282[医药卫生—中药学]