摘要
目的:基于超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法(UPLC-Q-Orbitrap-MS),定性分析鹿角方中的化学成分及其组织分布。方法:采用ACQUITY UPLC®BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm),流动相0.1%甲酸水溶液(A)-甲醇(B)梯度洗脱(0~2 min,4%B;2~6 min,4%~12%B;6~38 min,12%~70%B;38~38.5 min,70%B;38.5~39 min,70%~95%B;39~43 min,95%B;43~43.1 min,95%~4%B;43.1~45 min,4%B),流速0.3 m L·min^(-1),柱温40℃,进样量5μL,采用电喷雾离子源(ESI),正负离子全扫模式采集数据,扫描范围m/z 100~1500,碰撞能量10、20、40 e V。通过保留时间、精确相对分子质量、二级质谱碎片离子等信息,结合自建数据库,与对照品及文献数据进行比对,对鹿角方中化学成分及组织分布进行分析。结果:从鹿角方中共鉴定或推测出260个化合物,包括黄酮类156个,萜类43个,香豆素类18个,有机酸类13个,苯乙醇类7个,生物碱类7个,其他类16个,其中68种通过对照品比对鉴定。组织分布结果显示,分别在血、心脏、肝脏、肾脏中检测到原型成分100、143、129和126个。结论:该研究对鹿角方中的化学成分及组织分布进行了较全面的分析鉴定,可为鹿角方及其处方饮片的质量控制、临床应用、药代动力学、药效物质基础研究提供科学依据。
Objective:To qualitatively analyze the chemical constituents and their tissue distribution in Lujiao formula based on ultra performance liquid chromatography-quadrupole-electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap-MS).Method:The separation was performed on an ACQUITY UPLC®BEH C_(18) column(2.1 mm×100 mm,1.7μm)with the mobile phase of 0.1%formic acid aqueous solution(A)-methanol(B)in a gradient elution(0-2 min,4%B;2-6 min 4%-12%B;6-38 min,12%-70%B;38-38.5 min,70%B;38.5-39 min,70%-95%B;39-43 min,95%B;43-43.1 min,95%-4%B;43.1-45 min,4%B),the flow rate was 0.3 mL·min^(-1) with the column temperature of 40℃and the injection volume of 5μL.The data were acquired by an electrospray ionization(ESI)in the full scanning mode of positive and negative ions,the scanning rang was set at m/z 100-1500,the collision energies were 10,20,40 eV.Retention time,precise relative molecular mass and secondary mass spectrometry fragment ions were used to identify the compounds in Lujiao formula and analyze their tissue distribution,combing with self-established database and comparing with standard substances and published literature data.Result:A total of 260 compounds,including 156 flavonoids,43 terpenoids,18 coumarins,13 organic acids,7 phenylethanoids,7 alkaloids and 16 others,were identified or hypothesized from Lujiao formula,68 of which were identified by comparison with standard substances.And the results of tissue distribution showed that 100,143,129 and 126 prototype components were detected in blood,heart,liver and kidney,respectively.Conclusion:The chemical composition of Lujiao formula and their tissue distribution were systematic analyzed,which can provide reference for the quality control,clinical application,pharmacokinetics and pharmacodynamic material basis of Lujiao formula and its medicinal materials.
作者
张建伟
刘伟
沈沁
刘力
ZHANG Jianwei;LIU Wei;SHEN Qin;LIU Li(Third Grade Laboratory of Traditional Chinese Medicine(TCM)Preparations,National Administration of TCM,Shuguang Hospital Affiliated to Shanghai University of TCM,Shanghai 201203,China)
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2024年第8期148-156,共9页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家自然科学基金青年项目(82104616)
国家自然科学基金面上项目(81573648)
国家“重大新药创制”科技重大专项(2010ZX09102-208)
上海中医药大学附属曙光医院四明基金项目(SGKJ-201711)。
关键词
鹿角方
淫羊藿
女贞子
补骨脂
山茱萸
陈皮
化学成分
组织分布
超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法(UPLC-Q-Orbitrap-MS)
Lujiao formula
Epimedii Folium
Ligustri Lucidi Fructus
Psoraleae Fructus
Corni Fructus
Citri Reticulatae Pericarpium
chemical composition
tissue distribution
ultra performance liquid chromatography-quadrupole-electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap-MS)
