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酢浆草的HPLC指纹图谱建立及2种有效成分的含量测定                                                               Δ


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        李小双    1,2* ,李 银 ,刘文静 ,王广成 ,郑 林 ,陈思颖 ,李勇军 (1. 贵州医科大学民族药与中药开发应用
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        教育部工程研究中心/省部共建药用植物功效与利用国家重点实验室,贵阳 550004;2. 贵州医科大学药学院,
        贵阳 550004;3. 贵州医科大学贵州省药物制剂重点实验室,贵阳 550004)
        中图分类号 R284          文献标志码 A           文章编号 1001-0408(2020)06-0656-05
        DOI   10.6039/j.issn.1001-0408.2020.06.04

        摘   要   目的:建立酢浆草的高效液相(HPLC)指纹图谱,并同时测定其中异牡荆素、当药黄素的含量。方法:采用HPLC法。色
        谱柱为ACE Excel-5-C18,流动相为甲醇-0.1%磷酸水溶液(梯度洗脱),流速为1 mL/min,柱温为35 ℃,检测波长为280 nm,进样量
        为 10 μL。以异牡荆素峰为参照,绘制 12 批酢浆草药材样品的 HPLC 指纹图谱,采用《中药色谱指纹图谱相似度评价系统(2012
        版)》进行相似度评价,确定共有峰。按上述色谱条件同法测定异牡荆素、当药黄素的含量。结果:12批酢浆草药材样品共有19个
        共有峰,相似度均大于0.89,同时指认异牡荆素、当药黄素2个共有峰。异牡荆素、当药黄素检测质量浓度的线性范围分别为3.91~
        117.36 μg/mL(r=0.999 4)、9.88~118.56 μg/mL(r=0.999 2);定量限分别为0.675、3.587 μg/mL;检测限分别为0.205、1.087 μg/mL;
        精密度、重复性、稳定性试验的 RSD 均小于 2%;加样回收率分别为 95.46%~99.10%(RSD=1.23%,n=6)、95.34%~101.23%
        (RSD=2.74%,n=6);平均含量分别为0.227~1.654、0.641~2.052 mg/g。结论:所建指纹图谱可用于酢浆草药材的质量控制;含
        量测定方法简便、准确,可用于同时测定其中2种成分的含量。
        关键词     酢浆草;高效液相色谱法;指纹图谱;异牡荆素;当药黄素;含量测定
        Establishment of HPLC Fingerprint and Content Determination of Two Components of Oxalis corniculata
        LI Xiaoshuang ,LI Yin ,LIU Wenjing ,WANG Guangcheng ,ZHENG Lin ,CHEN Siying ,LI Yongjun(1.
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        Engineering Research Center for the Development and Application of Ethnic Medicine and TCM/State Key
        Laboratory of Functions and Applications of Medicinal Plants,Guizhou Medical University,Guiyang 550004,
        China;2. School of Pharmacy,Guizhou Medical University,Guiyang 550004,China;3. Guizhou Provincial
        Key Laboratory of Pharmaceutics,Guizhou Medical University,Guiyang 550004,China)
        ABSTRACT    OBJECTIVE:To establish the HPLC fingerprints of Oxalis corniculata and to simultaneously determine the contents
        of isovitexin and swertisin. METHODS:HPLC method was adopted. The determination was performed on ACE Excel-5-C18 column
        with mobile phase consisted of methanol-0.1% phosphoric acid water(gradient elution)at the flow rate of 1 mL/min. The column
        temperature was 35 ℃ ,and detection wavelength was set at 280 nm. The sample size was 10 μ L. Using isovitexin peak as
        reference,HPLC fingerprints of 12 batches of sample were drawn. The similarity evaluation was performed by using Similarity
        Evaluation System of Chromatogram Fingerprint of TCM(2012 edition)to determine common peaks. The contents of isovitexin
        and swertisin were determined by same method of above chromatogram. RESULTS:There were 19 common peaks in HPLC
        chromatogram of 12 batches of O. corniculata,with the similarity above 0.89. Two common peaks including isovitexin and
        swertisin were identified. The linear range of two components were 3.91-117.36 μg/mL(r=0.999 4)and 9.88-118.56 μg/mL(r=
        0.999 2),respectively. The limits of quantitation were 0.675 and 3.587 μg/mL;the limits of detection were 0.205 and 1.087 μg/mL,
        respectively. RSDs of precision,stability and reproducibility tests were all lower than 2%. The recoveries were 95.46%-99.10%
        (RSD=1.23% , n=6), 95.34% -101.23%(RSD=2.74% , n=6), respectively. The average contents were 0.227-1.654,
        0.641-2.052 mg/g,respectively. CONCLUSIONS:Established fingerprints can be used for the quality control of O. corniculata;
        the content determination method is simple and accurate,and can be used for simultaneous determination of two components.
                                                            KEYWORDS      Oxalis corniculata; HPLC; Fingerprint;
            Δ 基金项目:国家自然科学基金资助项目(No.U1812403);中央
                                                            Isovitexin;Swertisin;Content determination
        引导地方科技发展专项项目(No. 黔科中引地〔2018〕4006);贵州省科
        技计划项目(No.黔科合平台人才〔2016〕5613,No.黔科合平台人才
        〔2016〕5677);贵州省教育厅青年科技人才成长项目(No .黔科合 KY
        字〔2018〕179);贵州医科大学学术新苗培养及创新探索专项项目(No.                   酢浆草为酢浆草科植物酢浆草(Oxalis corniculata
        黔科合平台人才〔2018〕5779-12)                               L.)的新鲜或干燥全草,又称酸咪咪 ,为贵州省少数民
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            *硕士研究生。研究方向:药效物质基础。E-mail:1406520401@
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                                                            族常用药材,具有清热利湿、凉血消肿等功效 。该药主
        qq.com
                                                            要分布于我国华北、华中、华南及西南等地区 。有研究
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            # 通信作者:教授,硕士生导师,博士。研究方向:药效物质基
        础。E-mail:liyongjun026@126.com                       发现,酢浆草主要含有黄酮类、酚酸类等成分                  [4-7] ,具有抗
        ·656  ·  China Pharmacy 2020 Vol. 31 No. 6                                   中国药房    2020年第31卷第6期
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