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KHR98中生物碱的鉴定与定量及HPLC-Q-TOF-MS中的裂解途径

Identification and Quantification of Alkaloid in KHR98 and Fragmentation Pathways in HPLC-Q-TOF-MS.

作者信息

Long Jiakun, Wang Yang, Xu Chen, Liu Tingting, Duan Gengli, Yu Yingjia

机构信息

Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University.

出版信息

Chem Pharm Bull (Tokyo). 2018 May 1;66(5):527-534. doi: 10.1248/cpb.c17-00710. Epub 2018 Mar 2.

DOI:10.1248/cpb.c17-00710
PMID:29503397
Abstract

Uncaria rhynchophylla is woody climber plant distributed mainly in China and Japan, the stems and hooks of which can be collected as "Gou-Teng" for the treatment of hyperpyrexia, epilepsy and preeclampsia. Fudan University first manufactured KHR98, the extract of Uncaria rhynchophylla. In order to study the active components and structural information of KHR98, we established a HPLC coupled with quadrupole time-of-flight (Q-TOF)-MS method for rapid analysis of alkaloids. In qualitative analysis, a total of eight compounds, including four known alkaloids and four unknown components, were detected and identified. The fragmentation behaviors, such as the fragment ion information and the fragmentation pathways of the eight components were summarized simultaneously, and the concentration of the above components was determined by HPLC-MS method. The quantitative method was proved to be reproducible, precise and accurate. This study shed light on the standardization and quality control of the KHR98 and provided a foundation for the further research on pharmacology, follow-up clinical research and New Drug Applications.

摘要

钩藤是一种木质藤本植物,主要分布于中国和日本,其茎和钩可作为“钩藤”入药,用于治疗高热、癫痫和子痫前期。复旦大学首次制备了钩藤提取物KHR98。为了研究KHR98的活性成分和结构信息,我们建立了一种高效液相色谱-四极杆飞行时间质谱(Q-TOF-MS)联用方法,用于快速分析生物碱。在定性分析中,共检测并鉴定出8种化合物,包括4种已知生物碱和4种未知成分。同时总结了这8种成分的碎片离子信息和裂解途径等裂解行为,并采用高效液相色谱-质谱法测定了上述成分的含量。该定量方法具有良好的重现性、精密度和准确性。本研究为KHR98的标准化和质量控制提供了依据,为进一步的药理学研究、后续临床研究及新药应用奠定了基础。

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