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 C18 column (150 mm×2.1 mm,1.7 μm) 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 C18(250 mm×4.6 mm, 3 μm) 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.
DING Ya-ting, QIU Hong-chun, YIN Shan, ZHENG Xin, HANG Tai-jun
. Establishment of a method of the related substances of budesonide extended release tablets and identification by LC-MS[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(10)
: 1796
-1805
.
DOI: 10.16155/j.0254-1793.2021.10.17
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