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目的:采用UPLC/Q-TOF-MS对桂枝茯苓胶囊入血成分进行定性分析,为该制剂的体内药效物质研究提供参考。方法:Poroshell 120 EC-C_(18)色谱柱(3 mm×100 mm,1.7μm),流动相乙腈(A)-0.1%甲酸水溶液(B)梯度洗脱(0~5 min,5%A;5~20 min,5%~17%A;20~28 min,17%~30%A;28~30 min,30%~58%A;30~40 min,58%~83%A;40~45 min,83%~88%A;45~50 min,88%A),流速0.4 m L·min~(-1),柱温35℃,进样量10μL。采用电喷雾离子源,负离子扫描,毛细管电压3.5k V,雾化气压力45 Pa,干燥气流速10 L·min~(-1),加热毛细管温度350℃,源内裂解电压145 V,质量数扫描范围m/z 100~1 200。结果:通过与空白生物样品和对照品的提取离子色谱图、质谱碎片裂解信息比对,初步鉴定出14个入血成分,包括13个原型成分和1个代谢产物(野樱苷)。结论:建立的UPLC/Q-TOF-MS可为桂枝茯苓胶囊入血成分的定性分析提供一种快速、简便、可靠的分析手段,为该制剂的药效物质基础研究奠定基础。
OBJECTIVE: To qualitatively analyze the blood components of Guizhi Fuling capsule by UPLC / Q-TOF-MS, and to provide a reference for the study of pharmacodynamic substances in vivo. METHODS: Poroshell 120 EC-C 18 column (3 mm × 100 mm, 1.7 μm) was used. The mobile phase consisted of gradient elution with acetonitrile-A 0.1% formic acid in water (0-5 min, 5% A; 5 to 20 min, 5 to 17% A, 20 to 28 min, 17 to 30% A, 28 to 30 min, 30 to 58% A, 30 to 40 min, 58 to 83% 45 min, 83% ~ 88% A; 45 ~ 50 min, 88% A) at a flow rate of 0.4 m L · min -1. The electrospray ionization source, negative ion scan, capillary voltage 3.5k V, atomizing gas pressure 45 Pa, drying gas flow rate 10 L · min -1, heating capillary temperature 350 ℃, source pyrolysis voltage 145 V, scanning mass number Range m / z 100 ~ 1 200. Results: Fourteen inflow components, including 13 prototype components and 1 metabolite (wild cherry glycosides), were preliminary identified through the comparison with the extracted ion chromatogram and mass fragment fragmentation information of blank biological samples and control samples. Conclusion: The established UPLC / Q-TOF-MS can provide a quick, simple and reliable analytical method for the qualitative analysis of the components of the blood of Guizhi Fuling capsule, and lay a foundation for the study of the pharmacodynamic substances of the preparation.