基于UFLC－IT－TOF MS分析技术的妇科再造丸化学成分研究

Analysis of Chemical Constituents in Fuke Zaizao Pill by Ultra Fast Liquid Chromatography－Ion Trap Time-of-flight Mass Spectrometry

中文关键词:妇科再造丸  超快速液相色谱－离子阱飞行时间质谱联用技术（UFLC－IT－TOF MS）  化学物质基础  质量评价  二次开发

Key Words:Fuke Zaizao pill  ultra fast liquid chromatography－ion trap－time-of-flight mass spectrometry（UFLC－IT－TOF MS）  chemical substance basis  quality evaluation  secondary development

中文摘要:大品种妇科再造丸由42味中药组成，对多种妇科疾病具有显著疗效。但其组方复杂，化学成分尚未被充分阐明，质量控制水平较低。该研究建立了一种采用超快速液相色谱－离子阱飞行时间质谱联用技术（UFLC－IT－TOF MS）快速鉴定妇科再造丸化学成分的方法，系统研究了其化学物质基础。采用COSMOSIL C18色谱柱（3.0 mm × 150 mm，2.6 μm）进行分离，以0.4%乙酸和乙腈为流动相梯度洗脱；采用电喷雾离子源（ESI）在正负离子模式下采集妇科再造丸MS1、MS2和MS3的碎片信息。通过推导质谱裂解规律，与对照品、文献数据和单味药材图谱比对等方式，共鉴定出155种化学成分，包括萜类成分47个，酚及酚酸类成分43个，黄酮类成分39个，生物碱类成分14个，苯酞类成分8个，其他类成分4个，其中133个成分首次在妇科再造丸中发现。该研究进一步阐明了妇科再造丸的化学成分组成，为其质量标准的提高及药效物质的阐明提供了丰富信息。

Abstract:Fuke Zaizao pill consists of forty-two herbs，which is commonly utilized in clinic therapy for gynecological diseases．However，Fuke Zaizao pill has complicated chemical compositions that have not been adequately clarified，and its quality control needs to be improved．In this paper，an ultra fast liquid chromatography－ion trap time-of-flight mass spectrometry（UFLC－IT－TOF MS） was developed for rapid analysis of the chemical constituents in Fuke Zaizao pill．The gradient elution was performed on a COSMOSIL C18 column（3.0 mm × 150 mm，2.6 μm） with 0.4% acetic acid and acetonitrile as mobile phases．Positive and negative ion ESI modes were used simultaneously to collect MS1，MS2 and MS3 fragment information of Fuke Zaizao pill．A total of 155 chemical constituents were tentatively identified by deducing the mass spectrometric cleavage pattern，and comparing with standards，references and single herb chromatography，including 47 terpenoids，43 phenols and phenolic acids，39 flavonoids，14 alkaloids，8 phthalides，and 4 other structures，of which 133 components were firstly found in the Fuke Zaizao pill．The chemical composition of Fuke Zaizao pill was further elucidated in this paper，and a wealth of information for improving its quality standards and elucidating its effective components was provided.