超高效液相色谱-四极杆-飞行时间质谱法定性分析盐酸阿呋唑嗪中的杂质  

Qualitative analysis of impurities in alfuzosin hydrochloride by ultrahigh performance liquid chromatography-quadrupole-time of flight-mass spectrometry

作　　者：王军 邱荣英 李铁健 张贵民 WANG Jun;QIU Rong-ying;LI Tie-jian;ZHANG Gui-min(Shandong New Times Pharmaceutical Co.,Ltd.,Linyi Shandong 273400;National Engineering and Technology Research Center of Chirality Pharmaceutical,Linyi Shandong 273400;Lunan Pharmaceutical Group Co.,Ltd.,Linyi Shandong 276005)

机构地区：[1]山东新时代药业有限公司,山东临沂273400 [2]国家手性制药工程技术研究中心,山东临沂273400 [3]鲁南制药集团股份有限公司,山东临沂276005

出　　处：《中南药学》2021年第5期958-963,共6页Central South Pharmacy

摘　　要：目的建立超高效液相色谱-四极杆-飞行时间质谱法(UPLC-Q-TOF-MS)对盐酸阿呋唑嗪中的杂质进行定性分析。方法采用Thermo Hypersil gold aq C_(18)色谱柱,以10 mmol·L^(-1)乙酸铵水溶液与乙腈为流动相进行梯度分析,波长245 nm。质谱使用电喷雾离子源(ESI源),正离子模式检测,扫描范围m/z 50~800,雾化气温度300℃,干燥气流速10 L·min^(-1)。结果样品经过UPLC分离后,用Q-TOF-MS测定了6个杂质的精确分子量与质谱碎片离子,推测了杂质结构并分析了杂质来源。结论这6个杂质主要来自于合成过程,可为下一步的工艺优化与质量控制提供基础。Objective To qualitatively analyze the impurities in alfuzosin hydrochloride by ultrahigh performance liquid chromatography-quadrupole-time of flight-mass spectrometry(UPLC-Q-TOF-MS).Methods The chromatographic separation was performed on a Thermo Hypersil gold aq C_(18) column,with 10 mmol·L^(-1) ammonium acetate aqueous solution and acetonitrile as the mobile phase by gradient elution,and the wavelength was 245 nm.The MS was operated with an electrospray ionization(ESI)source and positive ion mode within a scanning range of m/z 50~800.The nebulizing temperature was set at 300℃and the dry gas flow was 10 L·min^(-1).Results The exact mass and fragment ions of 6 impurities were acquired by Q-TOF-MS after the separation by UPLC.The structure of the impurities were analyzed and the source of impurities was deduced.Conclusion The 6 impurities are generated mainly in the synthesis process,Which provides a reference for the optimization of the manufacturing and quality control of alfuzosin hydrochloride.

关 键 词：超高效液相色谱-四极杆-飞行时间质谱法 盐酸阿呋唑嗪 杂质结构 杂质来源 工艺优化 质量控制 

分 类 号：R927[医药卫生—药学]