Akademik Veri Yönetim Sistemi
JOURNAL OF CHEMICAL METROLOGY, cilt.19, sa.2, ss.199-208, 2025 (ESCI, Scopus)
A rapid ultra-performance liquid chromatographic method coupled with a quadrupole detector (UPLC-QDA) was developed and validated for the simultaneous determination of pinaverium bromide, medazepam, and their related substances in a newly developed fixed-dose pharmaceutical formulation. Chromatographic separation was achieved on an Acquity BEH C18 column (100 x 2.1 mm, 1.7 mu m) using a gradient elution of 25 mM ammonium formate buffer (pH 3.5) and acetonitrile at a flow rate of 0.6 mL/min and a column temperature of 45 degrees C. The total run time was 11 min, providing complete resolution of all analytes without interference. Linearity was demonstrated (R2 >= 0.999) within the ranges of 2-400 ng/mL for medazepam, 10-2000 ng/mL for pinaverium bromide, 5-1000 ng/mL for RS1 (medazepam impurity), and 10-2000 ng/mL for RS3-RS6 (pinaverium bromide impurities). The limits of detection (LOD) and quantitation (LOQ) were 0.17 and 0.50 ng/mL for medazepam and 0.43 and 1.30 ng/mL for pinaverium bromide, respectively, while LOD and LOQ values for related substances ranged between 0.22-0.91 ng/mL and 0.66-2.70 ng/mL. The method was validated in accordance with the ICH Q2(R2) guideline. The validated method was successfully applied for the simultaneous quantification of pinaverium bromide, medazepam, and their respective impurities (RS1-RS6) in commercial film-coated tablets (50 mg/10 mg), demonstrating its applicability for routine quality control and stability testing of fixed-dose combination formulations.