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川芎HPLC—APCI—MS特征图谱方法研究 被引量:2

Study on Composition Fingerprint of Ligusticum chuanxiong by HPLC-APCI-MS
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摘要 建立川芎中药高效液相色谱-大气压化学电离质谱(HPLC-DAD-APCI—MS)特征指纹图谱的分析方法。采用HPLC-DAD-APCI-MS联用技术,对川芎甲醇提取物中活性成分进行了分离和初步鉴定,并对10批不同来源的川芎样品和1批当归样品进行分析,建立川芎有效部位的特征图谱。本文所建立的色谱方法精密度、重现性、稳定性良好,采用APCI—MS共计鉴定出川芎甲醇提取物中10种有效成分,酚酸类化合物为:ferulic acid;苯酞类化合物:senkyunolide I、senkyunolide H、senkyunolide A、3-butylphthalide、coniferylferulate、Z-ligustilide、E—butyli—denephthalide;苯酞二聚体类化合物:riligustilide、levistolide A。该方法是川芎药材质量控制的可靠方法。 To establish a high performance liquid chromatographic fingerprinting method for the authentification and quality control of Ligusticum chuanxiong Hort. , high performance liquid chromatography (HPLC)-atmospheric pressure chemical ionization mass spectrometry (APCI-MS) has been applied to the analyzing active components in the methanol extract of Ligusticum chuanxiong Hort.. The separation was performed on a XDB-C18 (4.6 mm ×250 ram) column with gradient elution of methanol and water (with 0.1% acetic acid) at a flow-rate is 1 mL/min, under room temperature. Mutiple detectors including UV-VIS(DAD) ,and APCI-MS in both positive and negative mode have been used for compound identification. Ten major peaks of Ligusticum chuanxiong in the HPLC chromatogram have been tentative identified, and these include ferulic acid, senkyunolide I, senkyunolide H, senkyunolide A, 3 - butylphthalide, coniferylferu- late,Z-ligustilide, E-butylidenephthalide, riligustilide, and levistolide A. A reproducible HPLC fingerprinting method based on the distribution pattern and relative intensitives of 18 characteristic peaks has been established for authentification and qualify evaluation of Ligusticum chuanxiong.
出处 《天然产物研究与开发》 CAS CSCD 2007年第B05期12-17,共6页 Natural Product Research and Development
基金 国家自然科学基金项目(20235020) 共建生物医药研发测试中心项目(LS-05-KJZX-76)
关键词 川芎 高效液相色谱-大气压化学电离质谱 指纹图谱 Ligusticum chuanxiong Hort. PLC-APCI-MS fingerprint
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