Green and efficient preconcentration of calcium channel blocker drugs in water using effervescence powder in syringe-assisted deep eutectic solvent dispersive liquid-liquid microextraction

Abstract

Efficient preconcentration techniques are crucial for the analysis of calcium channel blocker drugs such as amlodipine and nifedipine, commonly used for hypertension and heart diseases. This study optimized the preconcentration conditions using CO2 effervescence powder assisted deep eutectic solvent dispersive liquid-liquid microextraction (EP-DLLME). A central composite design with 30 experiments was employed to determine the effects of extraction solvent volume, effervescence powder mass, water sample volume, and pH water. The optimized conditions for EP-DLLME were determined as follows: 500-μL of extraction solvent, 25-mL of water sample, 5 mg of effervescence powder, and pH 8. High-performance liquid chromatography (HPLC) coupled with a diode array detector was utilized for subsequent analysis. The method exhibited good linearity (r2 = 0.996) and low limits of detection and quantification: 1.73 ng/mL and 5.76 ng/mL for amlodipine, and 0.37 ng/mL and 1.23 ng/mL for nifedipine, respectively. The extraction efficiency, evaluated at three concentration levels, resulted in recoveries ranging from 73 % to 98 %. Repeatability analysis showed satisfactory intra-day and inter-day relative standard deviation values: 3.65 % to 8.38 % for amlodipine and 1.9 % to 10.11 % for nifedipine in the intra-day analysis, and 2.46 % to 9.07 % for amlodipine and 2.92 % to 10.7 % for nifedipine in the inter-day analysis. Furthermore, the EP-DLLME method demonstrated environmental sustainability, achieving a total AGREEnness score of 0.68, emphasizing its environmentally friendly nature.

Keywords

• Pharmaceutically active drug
• Microextraction
• Central composite design
• Greenness metric assessment