- Characterization of a novel process-related impurity in commercial bendazac lysine eye drops by LC-ESI-QTOF/MS/MS and NMR.
Characterization of a novel process-related impurity in commercial bendazac lysine eye drops by LC-ESI-QTOF/MS/MS and NMR.
Journal of pharmaceutical and biomedical analysis (2015-02-11)
Peixi Zhu, Weifeng Yang, Liya Hong, Qiaoyuan Cheng, Lei Luo, Jiajia He, Juanjuan Chen
PMID25666544
ABSTRACT
A simple and sensitive method was developed for characterization of two impurities from commercial bendazac lysine eye drops, by using liquid chromatography combined with electrospray ionization and QTOF mass analyzer (LC-ESI-QTOF MS/MS). A known impurity was characterized rapidly by comparison with the retention time and MS/MS data of the reference standard. Based on high resolution mass spectrometry (HRMS) and the nuclear magnetic resonance (NMR), a new impurity, purified by preparative HPLC, was identified as 2-(1,5-dibenzyl-1H-indazol-3-yloxy)acetic acid. In addition, a plausible mechanism for the formation of the impurities was also proposed.
MATERIALS
Product Number
Brand
Product Description
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
Supelco
Residual Solvent - Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetic acid, glacial, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, 99.8-100.5%
Sigma-Aldrich
Acetic acid, glacial, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8%
USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard