摘要
目的:建立超高效色谱法(UPLC法)测定布地奈德缓释片有关物质,并用液相色谱-四极杆-飞行时间串联质谱(LC-Q-TOF/MS)鉴定未知有关物质结构。方法:采用UPLC法,使用Waters ACQUITY UPLC BEH C;(150 mm×2.1 mm,1.7μm)色谱柱,以乙腈-磷酸盐缓冲溶液为流动相,梯度洗脱,对布地奈德缓释片有关物质进行分离;使用挥发性条件通过高分辨Q-TOF/MS测定未知有关物质的准确质量和元素组成,解析鉴定有关物质结构。采用液相色谱方法,使用Thermo BDS Hypersil C;(250 mm×4.6 mm,3μm)色谱柱,以乙腈-乙酸铵缓冲溶液为流动相,梯度洗脱,对布地奈德强降条件下产生的有关物质进行分离。结果:采用UPLC法时,主成分布地奈德及各有关物质分离度良好,并鉴定出6个未知有关物质,有关物质1和2为非对映异构体,有关物质3和4为差向异构体,有关物质5和10分别为文献中报道的布地奈德17-酸和布地奈德17-酮。结论:本文建立的方法简便、准确,专属性强,可用于布地奈德缓释片的有关物质检测和质量控制。
Objective:To establish and verify an UPLC method for related substances of budesonide extended release tablets and identified unknown related substances by LC-Q-TOF/MS.Methods:The separation was performed on a Waters ACQUITY UPLC BEH C;column(150 mm×2.1 mm,1.7μm)by linear gradient elution with a mobile phase consisting of acetonitrile-phosphate buffer.Volatile mobile phase was used for the determination of the accurate mass and elemental composition of parent ions of the product by Q-TOF/MS.The structures of the unknown related substances were then figured out through the elucidation of the fragment ions.The volatile separation was performed on a Thermo BDS Hypersil C;(250 mm×4.6 mm,3μm)by linear gradient elution with a mobile phase consisting of acetonitrile-ammonium acetate buffer.Results:Budesonide and its related substances could be separated well by UPLC.Six unknown related substances were identified.The unknow related substancecs 1 and 2 were identified as diastereomers.The unknow related substancecs 3 and 4 were identified as epimers,and the unknow related substancecs 5 and 10 were identified as budesonide 17-acid and budesonide 17-ketone having been reported before.Conclusion:The established method in this study is sample,accurate and specific for the examination and quality control of related substances of budesonide extended release tablets.
作者
丁亚婷
邱宏春
尹山
郑鑫
杭太俊
DING Ya-ting;QIU Hong-chun;YIN Shan;ZHENG Xin;HANG Tai-jun(China Pharmaceutical University,Nanjing 211198,China;Prinbury Biopharm Co.Ltd,Shanghai 201203,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2021年第10期1796-1805,共10页
Chinese Journal of Pharmaceutical Analysis
