UPLC-Q-Orbitrap HRMS结合HS-SPME-GC-MS技术的荆肤止痒颗粒化学成分分析  

Analysis on the chemical composition of Jingfuzhiyang Granules based on UPLC-Q-Orbitrap HRMS combined with HS-SPME-GC-MS technique

作　　者：谢易伶 鲍洋 田世民 蔡信福 李东 娄欣颖 马鸿雁[1] 张定堃[1,5] 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)

机构地区：[1]成都中医药大学药学院西南特色中药资源国家重点实验室,四川成都611137 [2]四川光大制药有限公司,四川彭州611930 [3]四川省抗病毒中药产业化工程技术研究中心,四川彭州611930 [4]国家中药现代化工程技术研究中心川药资源分中心,四川彭州611930 [5]成都中医药大学天府中医药创新港,四川省经典名方二次创新开发工程研究中心,四川成都611930

出　　处：《中国医院药学杂志》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)。

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.

关 键 词：荆肤止痒颗粒 UPLC-Q-Orbitrap HRMS HS-SPME-GC-MS 多组分表征 裂解规律 

分 类 号：R917[医药卫生—药物分析学]