超高效合相色谱串联四极杆飞行时间质谱在司盘组成分析方法中的应用研究  

Application of ultra-high performance convergence chromatography-tandem quadrupole time-of-flight mass spectrometry in the analysis of Span composition

作　　者：李樾[1,2] 许凯 杨锐 杨会英[1,2] LI Yue;XU Kai;YANG Rui;YANG Huiying(National Institutes for Food and Drug Control;NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients,Beijing 100050,China)

机构地区：[1]中国食品药品检定研究院 [2]国家药品监督管理局药用辅料质量研究与评价重点实验室,北京100050

出　　处：《中国药科大学学报》2024年第6期742-749,共8页Journal of China Pharmaceutical University

摘　　要：采用超高效合相色谱串联四极杆飞行时间质谱(UPCC-QTOF-MS)检测方法,建立定性分析药用辅料司盘组成的方法。采用VIRIDIS HSS C_(18)SB 100A色谱柱(3.0 mm×150 mm,18μm),以CO_(2)和异丙醇-四氢呋喃(98∶5)为流动相,梯度洗脱,柱温为50℃,流速为1 mL/min,以异丙醇-0.1%甲酸水溶液(8∶2)为补偿溶剂,背压为13.78 MPa,离子化模式为ESI^(+),采集模式为MS~E,扫描范围m/z 100~1200,分别测定司盘20、40、60、80、85样品。建立的方法可区分不同牌号司盘间组成差异,对各司盘组分进行定性分析,其中司盘20可分析得到21种组分,司盘40可分析得到7种组分,司盘60可分析得到13种组分,司盘80可分析得到9种组分,司盘85可分析得到9种组分,并根据各组分质谱图开展了结构分析。本研究建立的方法可区分不同牌号司盘间的组成差异,同时也可用于分析不同牌号的司盘组成及结构,此方法绿色环保,对司盘质量控制、工艺评价、制剂应用选择等具有指导意义。A method for the qualitative analysis of the composition of pharmaceutical excipient Span was established by ultra-high performance convergence chromatography-tandem quadrupole time-of-flight mass spectrometry(UPCC-QTOF-MS).The separation was performed on a VIRIDIS HSS C18 SB 100A column(3.0 mm×150 mm,18μm)with gradient elution using CO2 and isopropanol-tetrahydrofuran(98∶5)as the mobile phase.The column temperature was 50°C.The flow rate was 1 mL/min.Isopropanol and 0.1%formic acid aqueous solution(8∶2)were used as the compensation solvent.The back pressure was 13.78 MPa.The ionization mode was ESI+,the acquisition mode was MSE,and the m/z scanning range was from 100 to 1200.The samples of Span 20,40,60,80 and 85 were determined respectively.The established method could distinguish the composition differences between different brands of Span,and it could analyze the components of different brands of Span as well.21 components could be analyzed by Span 20,7 by Span 40,13 by Span 60,9 by Span 80,and 9 by Span 85,and the structural analysis of each component was carried out.The method established in this paper can distinguish the composition differences between different brands of Span.It can also be used to analyze the composition and structure of different brands of Span.This method is green and environmentally friendly with guiding significance for Span quality control,process evaluation,and preparation application selection,etc.

关 键 词：超高效合相色谱串联四极杆飞行时间质谱 司盘 组成分析 

分 类 号：R917[医药卫生—药物分析学]