Biological Safety Studies and Simultaneous Determination of Linagliptin and Synthetic Impurities by LC-PDA
Joint Authors
Ferreira, Flávio Dias
Oliveira, Luís Flávio Souza de
Machado, Michel Mansur
Paula, Fávero Reisdorfer
Duarte, Jonathaline Apollo
Heleno Ferreira, Raquel Balestri
Malesuik, Marcelo Donadel
Steppe, Martin
Schapoval, Elfrides Eva Shermann
Paim, Clésio S.
Source
Journal of Analytical Methods in Chemistry
Issue
Vol. 2019, Issue 2019 (31 Dec. 2019), pp.1-10, 10 p.
Publisher
Hindawi Publishing Corporation
Publication Date
2019-03-03
Country of Publication
Egypt
No. of Pages
10
Main Subjects
Abstract EN
A stability-indicating LC method was developed for quantification of linagliptin (LGT) and three synthetic impurities.
The method utilizes a Thermo Scientific® RP-8 column (100 mm × 4.6 mm; 5 μm) with the PDA detector for quantitation of impurities.
A mixture of 0.1% formic acid with pH 3.5 (A) and acetonitrile (B) was used as the mobile phase at a flow rate of 0.6 mL·min−1 with gradient elution.
The percentage of mobile phase B increases from 30% to 70% over 5 min and decreases from 70% to 30% between 5 and 8 min.
The method was validated according to International Council for Harmonization (ICH) guidelines.
The LOD values obtained were 0.0171 μg·mL−1 and 0.015 μg·mL−1 for LGT and impurities, respectively.
The LOQ values were 0.06 μg·mL−1 for LGT and impurities.
In all cases, the correlation coefficients of LGT and impurities were >0.999, showing the linearity of the method.
The % recovery of the LGT and added impurity were in the range of 92.92–99.79%.
The precision of the method showed values less than 1.47% for LGT and less than 4.63% for impurities.
The robustness was also demonstrated by small modifications in the chromatographic conditions.
The selectivity was evidenced because the degradation products formed in stress conditions did not interfere in the determination of LGT and impurities.
Toxicity prediction studies suggested toxicity potential of the impurities, which was confirmed using biological safety studies in vitro.
American Psychological Association (APA)
Heleno Ferreira, Raquel Balestri& Duarte, Jonathaline Apollo& Ferreira, Flávio Dias& Oliveira, Luís Flávio Souza de& Machado, Michel Mansur& Malesuik, Marcelo Donadel…[et al.]. 2019. Biological Safety Studies and Simultaneous Determination of Linagliptin and Synthetic Impurities by LC-PDA. Journal of Analytical Methods in Chemistry،Vol. 2019, no. 2019, pp.1-10.
https://search.emarefa.net/detail/BIM-1169264
Modern Language Association (MLA)
Heleno Ferreira, Raquel Balestri…[et al.]. Biological Safety Studies and Simultaneous Determination of Linagliptin and Synthetic Impurities by LC-PDA. Journal of Analytical Methods in Chemistry No. 2019 (2019), pp.1-10.
https://search.emarefa.net/detail/BIM-1169264
American Medical Association (AMA)
Heleno Ferreira, Raquel Balestri& Duarte, Jonathaline Apollo& Ferreira, Flávio Dias& Oliveira, Luís Flávio Souza de& Machado, Michel Mansur& Malesuik, Marcelo Donadel…[et al.]. Biological Safety Studies and Simultaneous Determination of Linagliptin and Synthetic Impurities by LC-PDA. Journal of Analytical Methods in Chemistry. 2019. Vol. 2019, no. 2019, pp.1-10.
https://search.emarefa.net/detail/BIM-1169264
Data Type
Journal Articles
Language
English
Notes
Includes bibliographical references
Record ID
BIM-1169264