西洛他唑有关物质的色谱-质谱结构鉴定
发布时间：2019-06-05 11:08
【摘要】：目的:采用色谱-质谱联用技术对西洛他唑有关物质进行结构鉴定。方法:采用Waters XTerra RP-8(100 mm×4.6mm,3.5μm)色谱柱串联Agilent Eclipse XDB-C8(12.5 mm×4.6 mm,5μm)保护柱,以水-乙腈为流动相梯度洗脱,流速为1.0 m L·min-1,检测波长为254 nm,对西洛他唑有关物质进行分离;采用电喷雾正离子化的方法,通过飞行时间质谱(TOF)测定一级质谱精确质量,三重四极杆/线性离子阱质谱(Q-TRAP)扫描二级与三级质谱,并进行结构解析。飞行时间质谱(TOF)和三重四极杆/线性离子阱质谱(Q-TRAP)的喷雾电压、雾化气压力、去溶剂温度依次分别为4 k V和5.5 k V、240 k Pa和275 k Pa、350℃和480℃。结果:西洛他唑与其有关物质分离良好,检测出8个有关物质,其中4个尚未见文献报道,并综合分析鉴定了有关物质结构。它们大部分具有6-[4-(1-环己基-1H-戊四唑-5-基)丁氧基-2(1H)-喹诺酮结构,制剂中有关物质状态与原料药中的相似。结论:色谱-质谱联用技术能有效地鉴定西洛他唑中有关物质,为其工艺和质量控制提供参考依据。
[Abstract]:Objective: to identify the structure of cilostazol related substances by chromatography-mass spectrometry. Methods: Waters XTerra RP-8 (100 mm 脳 4.6 mm, 3.5 渭 m) column was used in series Agilent Eclipse XDB-C8 (12.5 mm 脳 4.6 mm, 5 渭 m). The mobile phase was eluted with water-acetonitrile as mobile phase, and the flow rate was 1.0 mL 路min-1. The detection wavelength was 254 nm, for the separation of cilostazol related substances. The accurate mass of primary mass spectrometry was determined by time-of-flight mass spectrometry (TOF) by electrospray positive ionization method. Triple quadrupole / linear ion trap mass spectrometry (Q-TRAP) was scanned for secondary and tertiary mass spectrometry, and the structure of the mass spectrometry was analyzed. The spray voltage, atomization pressure and solvent removal temperature of time-of-flight mass spectrometry (TOF) and triple quadrupole / linear ion trap mass spectrometry (Q-TRAP) are 4kV and 5.5kV, 240k Pa and 275k Pa,350 鈩，
本文编号：2493483
[Abstract]:Objective: to identify the structure of cilostazol related substances by chromatography-mass spectrometry. Methods: Waters XTerra RP-8 (100 mm 脳 4.6 mm, 3.5 渭 m) column was used in series Agilent Eclipse XDB-C8 (12.5 mm 脳 4.6 mm, 5 渭 m). The mobile phase was eluted with water-acetonitrile as mobile phase, and the flow rate was 1.0 mL 路min-1. The detection wavelength was 254 nm, for the separation of cilostazol related substances. The accurate mass of primary mass spectrometry was determined by time-of-flight mass spectrometry (TOF) by electrospray positive ionization method. Triple quadrupole / linear ion trap mass spectrometry (Q-TRAP) was scanned for secondary and tertiary mass spectrometry, and the structure of the mass spectrometry was analyzed. The spray voltage, atomization pressure and solvent removal temperature of time-of-flight mass spectrometry (TOF) and triple quadrupole / linear ion trap mass spectrometry (Q-TRAP) are 4kV and 5.5kV, 240k Pa and 275k Pa,350 鈩，
本文编号：2493483
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