摘要
目的:采用色谱-质谱联用技术鉴定佐匹克隆的有关物质。方法:采用Phenomenex Luna 5u SCX 100A(250 mm×4.6 mm,5μm)色谱柱,以甲醇-乙腈-乙酸铵缓冲液为流动相,梯度洗脱,对佐匹克隆有关物质进行分离,采用电喷雾正离子化-飞行时间质谱法(ESI+-TOF/MS)测定各有关物质母离子的准确质量和元素组成,三重四极杆质谱测定子离子特征,结合对照品对照确定有关物质结构。结果:在所建立的条件下,佐匹克隆及其有关物质分离良好,检测并鉴定出7个主要有关物质。结论:色谱-质谱联用技术能有效地分离鉴定佐匹克隆中的有关物质,鉴定结果可为其质量控制和工艺优化提供参考依据。
Objective:To identify the related substances of zopiclone by LC-MS. Methods:The separation of zopiclone and its related substances was carried out on Phenomenex Luna 5u SCX 100A(250 mm×4.6 mm,5 μm)column using a mixture of methanol,acetonitrile,and ammonium acetate buffer as the mobile phase eluted with gradient program. The high resolution TOF/MS operated in ESI positive mode was used for the determination of the accurate mass and elemental composition of the parent ions of the related substances,and triple quadrupole tandem mass was employed for the product mass spectra determination. The structures of the related substances were then figured out through elucidation of the fragment ions and comparison with reference substances. Results:Zopiclone and its related substances were adequately separated under the established HPLC conditions. Seven major related substances of zopiclone were detected and identified by the hyphenated techniques. Conclusion:The established LC-MS method is effective for separation and identification of the related substances of zopiclone and the obtained results are suitable for the quality control and process optimization of zopiclone.
作者
汪澄
程方洁
陆宇婷
宋敏
杭太俊
WANG Cheng;CHENG Fang-jie;LU Yu-ting;SONG Min;HANG Tai-jun(Department of Pharmaceutical Analysis,China Pharmaceutical University,Nanjing 210009,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2019年第1期156-163,共8页
Chinese Journal of Pharmaceutical Analysis
