Objective： To identify the structure of related substances of urapidil injection. Methods： The separation of urapidil and its related substances was carried out on ACQUITY UHPLC® HSS C18（ 50 mm×2.1 mm, 1.7 μm） column,using 0.1% formic acid water and acetonitrile as the mobile phase,The quadrupole/electrostatic field orbitrap high-resolution mass spectrometry（ UHPLC-Q-Orbitrap HRMS） was used for detection. Combined with the precise relative molecular mass,fragmentation rule and chemical reaction theory,the structure of the relevant substances was speculated. Results： A total of 23 related substances were identified,which were mainly divided into 3 categories according to their sources：5 synthetic by-products（ related substances 1,6,15,19 and 22）,and 2 synthetic intermediates（related substances 5 and 7）,16 oxidative degradation products（ related substances 2-4,8-14,16-18,20-21,23） . The forced degradation test proved that urapidil was relatively stable to strong acids,strong alkali,high temperatures and light,while oxidation condition had a greater impact on urapidil. Conclusion： UHPLC-Q-Orbitrap HRMS technology can effectively identify the relevant substances in urapidil,which is significant for its production process optimization and quality control.
JIA Xue-dong, ZHANG Wan, SUN Zhi, LI Zhuo-lun, XUE Lian-ping, ZUO Li-hua, ZHOU Lin, DU Shu-zhang
. Structural identification of related substances in urapidil injection by HPLC-MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(7)
: 1226
-1236
.
DOI: 10.16155/j.0254-1793.2021.07.14
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