论文部分内容阅读
目的:建立液相色谱-二级质谱联用(LC-MS/MS)法对阿替洛尔片中的有关物质进行结构鉴定。方法:采用X-Bridge C18色谱柱(4.6 mm×250 mm,5μm),以0.1%三氟乙酸溶液-甲醇(90∶10)为流动相进行洗脱,LC-MS/MS法测定各有关物质的二级质谱,采用电喷雾离子源(ESI),正离子扫描模式,并对准分子离子的各个产物离子进行归属,对各杂质的可能结构进行推测。结果:阿替洛尔及其有关物质分离良好,共检测出4个有关物质,并进行定量和结构鉴定,其中2-(4-羟苯基)乙酰胺和2-4-[(2RS)-2,3-二羟丙氧基]苯基]乙酰胺2个有关物质为英国药典2015年版收载,2-4-[(RS)-2-羟丙氧基-3-氨基]苯基]乙酰胺和2-4-[(RS)-2-羟丙氧基,3-[N异丙基-N-乙酸)氨基)]苯基]乙酰胺2个有关物质未见报道。结论:本文所建立的LC-MS/MS法可以有效地分离分析阿替洛尔及其有关物质,对完善质量标准,加强药品质量控制具有重要意义。
OBJECTIVE: To establish a liquid chromatography-secondary mass spectrometry (LC-MS / MS) method for the identification of related substances in atenolol tablets. METHODS: The elution was carried out on a X-Bridge C18 column (4.6 mm × 250 mm, 5 μm) using 0.1% trifluoroacetic acid in methanol (90:10) as mobile phase. The related substances were determined by LC-MS / MS Of the second-order mass spectrometry, the use of electrospray ionization source (ESI), positive ion scan mode, and the molecular ions of each product ions belong to the speculation of the possible structure of the impurities. Results: Atenolol and its related substances were well separated. Four related substances were detected and quantified and identified. Among them, 2- (4-hydroxyphenyl) acetamide and 2-4 - [(2RS) 2,3-dihydroxypropoxy] phenyl] acetamide is contained in the edition of the British Pharmacopoeia 2015 edition, and 2 - [(RS) -2- hydroxypropoxy-3-amino] phenyl] Acetamide and two related substances of 2-4 - [(RS) -2-hydroxypropoxy, 3- [N-isopropyl-N-acetic acid) amino]] phenyl] acetamide have not been reported. Conclusion: The established LC-MS / MS method can effectively separate and analyze atenolol and its related substances, which is of great significance for improving quality standards and enhancing drug quality control.