基于UPLC-ESI-Q-TOF-MS/MS技术快速鉴定柴石退热颗粒的化学成分  

Identification of Chemical Constituents in Chaishi Tuire Granules by UPLC-ESI-Q-TOF-MS/MS

作　　者：杨丽[1] 袁丰瑞 曹岚[1] 段烨琳 邹萌 张勇[1] 何军伟 YANG Li;YUAN Feng-rui;CAO Lan;DUAN Ye-lin;ZOU Meng;ZHANG Yong;HE Jun-wei(Jiangxi University of Chinese Medicine,Nanchang 330004,China;Sinopharm Group Guangdong Medi-world Pharmaceutical Co.Ltd.,Foshan 528000,China)

机构地区：[1]江西中医药大学,南昌330004 [2]国药集团广东环球制药有限公司,广东佛山528000

出　　处：《中国实验方剂学杂志》2021年第17期152-159,共8页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国药集团广东环球制药有限公司委托项目。

摘　　要：目的:采用超高效液相色谱-电喷雾/四极杆飞行时间串联质谱法(UPLC-ESI-Q-TOF-MS/MS)技术快速鉴定柴石退热颗粒的化学成分。方法:采用Phenomenex Luna omega C18色谱柱(2.1 mm×100 mm,1.6μm),以0.1%甲酸水溶液(A)-乙腈(B)为流动相进行梯度洗脱(0~20 min,5%~40%B;20~40 min,40%~95%B;40~43 min,95%B),流速0.3 mL·min^(-1),采用电喷雾离子源(ESI),在正、负离子模式下采集数据,扫描范围m/z 150~1 500,通过与对照品的保留时间及质谱数据信息对比,并结合精确相对分子质量、质谱裂解规律、质谱数据库(PubChem,MassBank,ChemicalBook等)及相关文献,对柴石退热颗粒的化学成分进行快速鉴定,并明确各成分的药材归属。结果:共鉴定了85个化学成分,包括28个黄酮类,24个苯丙素类,11个萜类,10个生物碱类,4个醌类及8个其他类;其中19个化合物来源于金银花,14个化合物来源于黄芩,10个化合物来源于板蓝根,9个化合物来源于蒲公英,9个化合物来源于连翘,4个化合物来源于柴胡,4个化合物来源于知母,4个化合物来源于大黄。结论:柴石退热颗粒含有丰富的化学成分且来源于多味药材,为其质量控制、物质基础及体内代谢分析奠定了研究基础。Objective:To rapidly identify the chemical constituents of Chaishi Tuire granules by ultraperformance liquid chromatography-electrospray/quadrupole time-of-flight tandem mass spectrometry(UPLCESI-Q-TOF-MS/MS). Method: Chromatographic separation was conducted on a Phenomenex Luna omega C18 column(2.1 mm×100 mm,1.6 μm)with 0.1% formic acid aqueous solution(A)-acetonitrile(B)as the mobile phases for gradient elution(0-20 min,5%-40%B;20-40 min,40%-95%B;40-43 min,95%B),the flow rate was set at 0.3 mL·min^(-1). MS data were collected in positive and negative ion modes,the scanning range was m/z150-1 500 and electrospray ionization(ESI)was employed. The chemical constituents of Chaishi Tuire granules were identified by comparing with the retention time and the mass data of the reference substances,as well as the accurate mass,MS/MS fragment ions,mass spectrometry databases(PubChem,MassBank,ChemicalBook and others) and related literature. Result: A total of 85 chemical constituents were identified, including 28 flavonoids,24 phenylpropanoids,11 terpenoids,10 alkaloids,4 quinones,and 8 others. Among them,19 constituents derived from Lonicerae Japonicae Flos, 14 constituents derived from Scutellariae Radix, 10 constituents derived from Isatidis Radix,9 constituents derived from Taraxaci Herba,9 constituents derived from Forsythiae Fructus,4 constituents derived from Bupleuri Radix,4 constituents derived from Anemarrhenae Rhizoma,and 4 constituents derived from Rhei Radix et Rhizoma. Conclusion: Chaishi Tuire granules is rich in phytochemicals, which are derived from many of traditional Chinese medicines. This study can lay a foundation for the quality control,material basis and in vivo metabolic analysis of this preparation.

关 键 词：柴石退热颗粒 超高效液相色谱-电喷雾/四极杆飞行时间串联质谱法(UPLC-ESI-Q-TOF-MS/MS) 黄酮类 苯丙素类 萜类 生物碱类 裂解规律 

分 类 号：R22[医药卫生—中医基础理论] R28[医药卫生—中医学]