首页|基于传统分离和UHPLC-Q-Orbitrap HRMS技术的狗脊饮片化学成分分析

基于传统分离和UHPLC-Q-Orbitrap HRMS技术的狗脊饮片化学成分分析

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目的:系统分析狗脊饮片的化学成分。方法:利用正反相硅胶、聚酰胺和葡聚糖凝胶Sephadex LH-20等分离手段对狗脊饮片70％乙醇提取物进行分离纯化，根据1H-NMR和13C-NMR数据鉴定其结构;进一步采用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱技术(UHPLC-Q-Orbitrap HRMS)对狗脊饮片化学成分进行分析，以ACQUITY UPLC BEH C18(2。1 mm× 100 mm，1。7 μm)为色谱柱，乙腈-0。1％甲酸水为流动相进行梯度洗脱;正负离子模式下采集质谱数据。结果:共分离得到8个单体化合物，其中化合物C1为首次从狗脊饮片中分离得到;基于UHPLC-Q-Orbitrap HRMS技术，根据精确分子质量、保留时间、碎片离子等信息共分析42个化合物，包括18个苯丙素、8个酚酸、4个蕨素、3个酚类、4个芳香族、1个黄酮和4个其他化合物。结论:该研究首次结合传统分离手段和UHPLC-Q-Orbitrap HRMS技术较为全面地分析了狗脊饮片化学成分，为该药材血清药物化学、药动学和质量控制研究提供部分参考。
Chemical constituents of processed Cibotium barometz analyzed by traditional separation technology and UHPLC-Q-Orbitrap HRMS method
OBJECTIVE To systematically analyze the chemical constituents of processed Cibotium barometz.METHODS The chemical constituents from the 70％ethanol extract of processed C.barometz were isolated by silica gel,poly-amide column,and Sephadex LH-20.The isolated compounds were identified according to the 1H-NMR and 13C-NMR data.Fur thermore,an ultra-high performance liquid chromatography coupled with quadrupole orbitrap high-resolution mass spectrometry technology(UHPLC-Q-Orbitrap HRMS)was utilized to qualitatively analyze the constituents from processed C.barometz.An ACQUITY UPLC BEH C18(2.1 mm× 100 mm,1.7 μm)column was used as the analytical column eluted with acetonitrile(A)and 0.1％aqueous formic acid(B)in a gradient elution program.The mass data were acquired both in positive and negative ion modes.RESULTS Totally 8 compounds were isolated from processed C.barometz.Compound C1 was obtained from this plant for the first time;a total of 42 compounds were identified and characterized by UHPLC-Q-Orbitrap HRMS including 18 phenyl-propanoids,8 phenolic acids,4 pterosins,3 phenolics,4 aromatics,1 flavonoid and 4 others according to their accurate molecular mass,retention times and fragmentation ion information.CONCLUSION Traditional separation technologies and UHPLC-Q-Orbitrap HRMS method were integrated to comprehensively analyze the chemical constituents of processed C.barometz for the first time.The results of this study provide reference for the further research on the serum pharmacochemistry,pharmacokinetics and quality control of C.barometz.

processed Cibotium barometztraditional separationUHPLC-Q-Orbitrap HRMSchemical constituents

曾凡丽、李朋飞、王倩、蔡海敏、冉俊艳、廖尚高、罗喜荣、关焕玉

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贵州医科大学药学院/省部共建药用植物功效与利用国家重点实验室,贵州贵阳 550025

贵州省人民医院国家药物临床试验机构,贵州贵阳 550002

狗脊饮片 传统分离 UHPLC-Q-Orbitrap HRMS 化学成分

贵州省科技计划项目贵州省科技计划项目贵州省卫生健康委科学技术基金贵州医科大学教学改革研究项目

黔科合基础[2020]1Y374黔科合基础ZK[2021]一般531gzwkj2021-443JG2021046

2024

10.13286/j.1001-5213.2024.03.04

中国医院药学杂志
中国药学会

中国医院药学杂志

CSTPCD北大核心
影响因子：1.198
ISSN：1001-5213
年,卷(期)：2024.44(3)
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