Related substances in empagliflozin determined by LC-MS/MS
10.13220/j.cnki.jipr.2016.04.032
- Author:
Hao ZHOU
1
Author Information
1. Department of Traditional Chinese Materia Medica, Shenyang Pharmaceutical University
- Publication Type:Journal Article
- Keywords:
Content;
Empagliflozin;
Impurity;
LC-MS/MS
- From:
Journal of International Pharmaceutical Research
2016;43(4):753-756
- CountryChina
- Language:Chinese
-
Abstract:
Objective: To develop a LC-MS/MS method for the quantification of empagliflozin (EPLZ) impurity X(EPLZ-X) in EPLZ pharmaceutical product. Methods: Isocratic chromatographic separation was performed on a Thermo BDS C18 column (4.6 mm × 100 mm,2.4mm). The mobile phase consisting of acetonitrile-water(75: 25, V/V) was eluted at a flow rate of 0.7 ml/min. ESI source was applied and operated in the positive ion mode. multiple reaction monitoring(MRM) mode with the transitions of m/z 785→m/z 475 and m/z 785→m/z 418 were used to quantify the EPLZ-X. Results: The method was linar in the concentration range from 0.5 to 100.6 ng/ml. The limit of quantification was 0.5 ng/ml. The intra-and inter-day precision values were both below 11.8%, and accuracy was within ±2.5% in all quality control samples. The average recovery was 105.1%,109.8% and 102.6%, respectively. Conclusion: The method provides a sensitive and specific means for the determination of EPLZ-X in EPLZ pharmaceutical substances and completely meets the requirement of European Medicines Evaluation Agency(EMEA) (a limit of not more than 60×10-6 g for the mutagenic impurity EPLZ-X).
