Ultra-Performance Liquid Chromatographic and Densitometric Methods for Sensitive Determination of Xipamide and Triamterene in Pure and Pharmaceutical Dosage Forms

BACKGROUND: Validated ultra-performance liquid chromatography (UPLC) and thin-layer chromatography (TLC) densitometric methods were prescribed for determination of antihypertensive components. OBJECTIVE: To establish and validate rapid and accurate UPLC and TLC densitometric methods for determination of Xipamide and Triamterene in pure and dosage forms. METHODS: The first method, UPLC, depended on using an Agilent Zorbax Eclipse Plus C8 (50 mm × 2.1 mm, 1.8 μm) column, a mobile phase composed of acetonitrile-water (70 + 30, v/v) adjusted by acetic acid to obtain pH 3, 0.2 mL/min flow rate, and UV detection at 231.4 nm. The second method was a TLC densitometric method. Separation was achieved by using toluene-methanol-ethyl chloride-acetic acid (7 + 2 + 1 + 0.2, v/v/v) as the mobile phase, pre coated silica gel plates as the stationary phase, and UV detection at 300.0 nm. RESULTS: The obtained results were validated and statistically compared with official and reported methods. The obtained results showed high accuracy and reproducible results with excellent mean recoveries for both drugs. CONCLUSION: The UPLC method showed shorter retention time for both Xipamide (0.88 min) and Triamterene (0.63 min), a lower detection limit of less than 0.055 µg/mL for both drugs with high selectivity, decreased injection volume (1 µL), and a lower flow rate than any HPLC method. Both proposed methods were sensitive, selective, and effectively applied to pure and dosage forms (Epitens®). HIGHLIGHTS: Unprecedented sensitive, rapid, and reproducible UPLC and TLC methods were developed for selective determination of mixtures of Xipamide and Triamterene, with LOD os less than 0.076 µg/mL for both drugs.