摘要
目的:利用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap HRMS)和顶空-固相微萃取气质联用(HS-SPME-GC-MS)技术分析荆肤止痒颗粒的醇溶性及挥发性化学成分,解析化合物裂解规律,揭示制剂中的成分归属,完善中药制剂的质量标准。方法:UPLC-Q-Orbitrap HRMS采用Thermo Scientific Accucore^(TM)C_(18)(3 mm×100 mm,2.6μm)色谱柱,以0.1%甲酸水溶液(A)-甲醇(B)为流动相进行梯度洗脱,正、负离子模式下采集数据。根据精准质荷比和二级碎片离子信息,结合文献数据库对荆肤止痒颗粒的醇溶性成分进行鉴定。采用HS-SPME-GC-MS鉴定荆肤止痒颗粒中的挥发性成分,将色谱峰信息与标准数据库进行检索对比,对荆肤止痒颗粒的挥发性成分进行快速鉴定。结果:从荆肤止痒颗粒中共鉴定出162个化合物,其中从UPLC-Q-Orbitrap HRMS结果中鉴定出129个醇溶性化合物,包括黄酮类35个、香豆素类10个、生物碱类3个、有机酸类39个、氨基酸类12个、酰胺类6个、核苷类6个和其他类18个;从HS-SPME-GC-MS结果中鉴定出33个挥发性化合物,包括烃类7个、醛类12个、酮类3个、酯类3个、有机酸类4个、醇类2个和杂环2个。结论:建立了荆肤止痒颗粒的UPLC-Q-Orbitrap HRMS和HS-SPME-GC-MS分析方法,为阐明该复方制剂的药效物质基础提供了依据,可为进一步完善质量标准、优化工艺、稳定药效提供参考。
OBJECTIVE To analyze the alcohol-soluble and volatile constituents of Jingfuzhiyang Granules by ultra-high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap HRMS)and headspace solid-phase microextraction-gas chromatography-mass spectrometry(HS-SPME-GC-MS)for analyzing the cleavage pattern of the compounds,reveal the attribution of the constituents in the preparation and improve the quality standard of Chinese medicinal preparations.METHODS UPLC-Q-Orbitrap HRMS analysis was performed on a Thermo Scientific Accucore^(TM)C_(18)(3 mm×100 mm,2.6μm)ultra-performance liquid column.The mobile phase was a gradient elution of 0.1%formic acid aqueous solution(A)-methanol(B).MS data were collected in positive and negative ion modes.The alcohol-soluble constituents of Jingfuzhiyang Granules were identified on the basis of accurate mass charge ratios and secondary fragmentation ion information and in conjunctions with the literature data.HS-SPME-GC-MS analysis was utilized for identifying the volatile constituents in Jingfuzhiyang Granules and chromatographic peak information was acquired and compared with the standard database for a rapid identification of volatile constituents.RESULTS Totally 162 chemical constituents were identified in Jingfuzhiyang Granules,among which 129 alcohol-soluble compounds were identified from the results of UPLC-Q-Orbitrap HRMS,including 35 flavonoids,10coumarins,3 alkaloids,39 organic acids,12 amino acids,6 amides,6 nucleosides and 18 others;33 volatile compounds were identified from the results of HS-SPME-GC-MS,including 7 hydrocarbons,12 aldehydes,3 ketones,3 esters,4 organic acids,2 alcohols and 2 heterocycles.CONCLUSION The analytical protocol of UPLC-Q-Orbitrap HRMS and HS-SPME-GC-MS has been formulated for elucidating pharmacological substance basis of compound preparation,providing references for further improving the quality,optimizing the process and stabilizing the pharmacological effect.
作者
谢易伶
鲍洋
田世民
蔡信福
李东
娄欣颖
马鸿雁
张定堃
XIE Yiling;BAO Yang;TIAN Shimin;CAI Xinfu;LI Dong;LOU Xinying;MA Hongyan;ZHANG Dingkun(State Key Laboratory of Southwestern Chinese Medicine Resources,School of Pharmacy,Chengdu University of Traditional Chinese Medicine,Sichuan Chengdu 611137,China;Sichuan Guangda Pharmacy Company Limited,Sichuan Pengzhou 611930,China;Sichuan Engineering Research Center of Antiviral Traditional Chinese Medicine Industrialization,Sichuan Pengzhou 611930,China;Sichuan Herbal Resources Sub-center of National Engineering Research Center for Modernization of Traditional Chinese Medicine,Sichuan Pengzhou 611930,China;Sichuan Provincial Engineering Research Center of Innovative Re-development of Famous Classical Formulas,Tianfu TCM Innovation Harbor,Chengdu University of Traditional Chinese Medicine,Sichuan Chengdu 611930,China)
出处
《中国医院药学杂志》
CAS
北大核心
2024年第21期2484-2491,共8页
Chinese Journal of Hospital Pharmacy
基金
四川省科技计划资助项目(编号:2022YFS0429)。
作者简介
谢易伶,女,硕士,研究方向:中药质量控制与评价;通信作者:马鸿雁,女,博士,副教授,研究方向:中药质量控制与评价;通信作者:张定堃,男,博士,副教授,研究方向:中药制剂新技术与质量评价。
