[关键词]
[摘要]
目的 对栝楼桂枝汤进行血清药物化学成分研究,阐明其体内药效物质基础。方法 通过高效液相串联飞行时间质谱(HPLC-Q-TOF-MS)法快速鉴定栝楼桂枝汤经大鼠ig给药后吸收入血的化学成分。HPLC-Q-TOF-MS法采用Shimadzu Inertsil ODS-SP(250 mm×4.6 mm,5 μm)色谱柱,以乙腈-0.1%甲酸水为流动相进行梯度洗脱,采用负离子模式扫描,对空白血清、大鼠ig栝楼桂枝汤后的含药血清以及栝楼桂枝汤提取原液进行对比分析,确定血中移行成分。结果 通过比较色谱峰保留时间、质谱信息、质谱裂解方式,共确认了栝楼桂枝汤42个吸收入血成分,包括单萜苷类、黄酮类、酚酸类、姜酚类、三萜皂苷类及没食子酰糖类等。结论 建立的HPLC-Q-TOF-MS鉴定栝楼桂枝汤血清药物化学成分的分析方法简便、快速、准确,为揭示栝楼桂枝汤对脑卒中后康复,在体内发挥神经保护作用的药效物质提供实验依据。
[Key word]
[Abstract]
Objective To study the serum pharmacochemistry of Gualou Guizhi Decoction (GLGZD) as well as the material basis through analyzing the constituents absorbed in blood. Methods A high performance liquid chromatography-quadrupole-time- of-flight mass spectrometry (HPLC-Q-TOF-MS) method was developed for the analysis on absorbed components in serum after ig administration of GLGZD to rats. The separation was achieved on a C18 column by gradient elution with acetonitrile-aqueous solution (containing 0.1% formic acid) as mobile phase. The ion acquisition was performed by full scan MS and MS/MS in negative ion mode.The serum after ig administration of GLGZD to rats, blank serum of rats, and GLGZD extracts sample were analyzed by HPLC-Q-TOF-MS. Results Forty-two prototype compounds including monoterpene glycosides, flavonoids, phenolic acids, gingerols, triterpenoid saponins, galloylglucoses, and others were confirmed and identified in serum by comparing the retention time and mass spectrometry fragmentation characteristics with reference standards or literatures. Conclusion The analysis of absorbed components of GLGZD in serum after administration by serum pharmacochemistry method would provide an experimental basis for revealing the real neuroprotective constituents of GLGZD in treating dysfunction after stroke.
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[基金项目]
国家自然科学基金资助项目(81503204,81674046,81673561);福建中医药大学校管课题(X2015015,X2014109,X2014132);福建省高校新世纪优秀人才支持计划(闽教科2015);福建省高校杰出青年科研人才计划(闽教科2016)