Simple, Accurate and Multianalyte Determination of Thirteen Active Pharmaceutical Ingredients in Polypills by HPLC-DAD

Abstract

A new universal HPLC-DAD method has been developed for the separation and simultaneous determination of thirteen active pharmaceutical ingredients (APIs): ramipril, lisinopril, enalapril; atenolol, metoprolol; losartan, candesartan; rosuvastatin, atorvastatin, simvastatin; amlodipine; hydrochlorothiazide, acetylsalicylic acid in polypills used in the treatment of hypertension. The chromatographic analysis of the APIs was performed on an ACE-5 C18-PFP column (250 mm × 4.6 mm, 5 μm) with 0.01 M phosphate buffer (pH = 2.50) and acetonitrile in gradient elution as the mobile phase at a flow rate 1.0 mL min−1. UV detection was performed at 230 nm. The analysis time was 35 min. The elaborated method meets the acceptance criteria for specificity, linearity, sensitivity, accuracy, and precision for all examined substances. The linearity range was observed in a wide concentration range, whereas the determination coefficients (R2) for the linear model were greater than 0.990. The sensitivity of the method was good with the LOD and LOQ values ranged from 0.0009 to 0.0923 mg mL−1 and from 0.0027 to 0.2794 mg mL−1, respectively. The proposed method showed good precision with RSD less than 1.91% and the accuracy expressed as percent recovery was from 95.20% to 104.62%. The proposed HPLC-DAD method was successfully applied to determine APIs in prepared model mixtures corresponding to the commercially available polypill tablets. The obtained results of the measured contents were with good accuracy (95.84–103.92%) and high precision (RSD < 0.95%) indicating the applicability of the proposed method for the simultaneous determination of the polypill components. Therefore, the method can be an effective tool in the quality control of polypills.

Keywords

• polypills
• active pharmaceutical ingredients
• quantitative analysis
• HPLC-DAD