Characterization and quantitative determination of impurities in piperaquine phosphate by HPLC and LC/MS/MS.
Four impurities in piperaquine phosphate bulk drug substance were detected by a newly developed gradient reverse phase high performance liquid chromatographic (HPLC) method. These impurities were identified by LC/MS/MS. The structures of impurities were confirmed by spectroscopic studies (NMR and IR) conducted using synthesized authentic compounds. The synthesized reference samples of the impurity compounds were used for the quantitative HPLC determination. The system suitability of HPLC analysis established the validity of the separation. The method was validated according to ICH guidelines with respect to specificity, precision, accuracy and linearity. Forced degradation studies were also performed for piperaquine phosphate bulk drug samples to demonstrate the stability indicating power of the newly developed HPLC method.
Dongre
Vaijanath G
VG
Department of Chemistry, University of Mumbai, Vidyanagari, Kalina, Santacruz (East), Mumbai 400098, India. dongrevg@yahoo.com
Karmuse
Pravin P
PP
Ghugare
Pradeep D
PD
Gupta
Mukesh
M
Nerurkar
Bipin
B
Shaha
Chirag
C
Kumar
Ashok
A
D002851:Chromatography, High Pressure Liquid; D004340:Drug Contamination; D007202:Indicators and Reagents; D009682:Magnetic Resonance Spectroscopy; D013058:Mass Spectrometry; D011804:Quinolines / Q000032:analysis*; D013055:Spectrophotometry, Infrared; D013056:Spectrophotometry, Ultraviolet; D010879:Piperazines
D007202:Indicators and Reagents; D011804:Quinolines; C034759:piperaquine; D010879:Piperazines