Event Title

Quantitative analysis of cetirizine dihydrochloride by HPLC (high performance liquid chromatography) and q-NMR (quantitative nuclear magnetic resonance) techniques

Location

D1497

Start Date

4-12-2019 10:10 AM

End Date

4-14-2019 10:40 AM

Abstract

The pharmaceutical industry mainly uses HPLC and gas chromatography (GC), for quantitative analysis of the active ingredients. Quantitative proton-nuclear magnetic resonance technique (q-NMR) provides an alternative method for quantification of these drugs and a wide variety of other organic compounds. In this study comparative quantitative analyses of cetirizine dihydrochloride were conducted by HPLC and q-NMR techniques. Concentrations range of 0.043 mM to 0.22 mM were used for HPLC analysis. Plackett-Burman design of experiment (DOE) approach was employed for screening and optimization of buffer concentration, organic solvent percentage, and injection volume. Box Behnken design was utilized for further optimization. The optimal conditions found from DOE were 2.1 pH 40 mM phosphate buffer with acetonitrile 22:78 v/v as the mobile phase at a flow rate of 2 mL/min, and an injection volume of 5mL. These optimal conditions resulted in 4% deviation in retention time from the predicted value. Validation studies of the HPLC method showed high degree of linearity (regression value of 0.9994), accuracy, robustness, and stability. The q-NMR studies were done on 300 MHz NMR instrument using maleic acid as the internal standard. Cetirizine dihydrochloride in D2O solutions with concentrations range of 20-100 mM with 50 mM of maleic acid were analyzed in triplicate. The peak area of three sets of protons in cetirizine were quantified with respect to the olefinic protons peak area of maleic acid. The calibration curves of peak areas vs. concentrations for three different sets of protons showed linear relationship with regression values of greater than 0.998.

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Apr 12th, 10:10 AM Apr 14th, 10:40 AM

Quantitative analysis of cetirizine dihydrochloride by HPLC (high performance liquid chromatography) and q-NMR (quantitative nuclear magnetic resonance) techniques

D1497

The pharmaceutical industry mainly uses HPLC and gas chromatography (GC), for quantitative analysis of the active ingredients. Quantitative proton-nuclear magnetic resonance technique (q-NMR) provides an alternative method for quantification of these drugs and a wide variety of other organic compounds. In this study comparative quantitative analyses of cetirizine dihydrochloride were conducted by HPLC and q-NMR techniques. Concentrations range of 0.043 mM to 0.22 mM were used for HPLC analysis. Plackett-Burman design of experiment (DOE) approach was employed for screening and optimization of buffer concentration, organic solvent percentage, and injection volume. Box Behnken design was utilized for further optimization. The optimal conditions found from DOE were 2.1 pH 40 mM phosphate buffer with acetonitrile 22:78 v/v as the mobile phase at a flow rate of 2 mL/min, and an injection volume of 5mL. These optimal conditions resulted in 4% deviation in retention time from the predicted value. Validation studies of the HPLC method showed high degree of linearity (regression value of 0.9994), accuracy, robustness, and stability. The q-NMR studies were done on 300 MHz NMR instrument using maleic acid as the internal standard. Cetirizine dihydrochloride in D2O solutions with concentrations range of 20-100 mM with 50 mM of maleic acid were analyzed in triplicate. The peak area of three sets of protons in cetirizine were quantified with respect to the olefinic protons peak area of maleic acid. The calibration curves of peak areas vs. concentrations for three different sets of protons showed linear relationship with regression values of greater than 0.998.