<p>The quantitative nuclear magnetic resonance (qNMR) method of quantifying the content of pharmaceuticals is an important and growing science in the current era. The deuterium-based solvents contribute to the main costs of the NMR-based analysis. In this study, we introduced the use of deuterium-free solvent (i.e., water H<sub>2</sub>O) for the quantification of ciprofloxacin (CIP) using the qNMR method. <i>p</i>-Nitrophenol (PNP) was used as an internal standard to solve the absolute integration of signals in NMR spectra. Quantification results were compared with literaturereported high-performance liquid chromatographic (HPLC) methods and analyzed by analysis of variance (ANOVA). The ANOVA results show that the regression model is highly significant (<i>F</i> = 37515.62, <i>p</i> &lt; 0.001), indicating that the actual quantity of the analyte is a powerful predictor of the quantized concentration. An ANOVA study demonstrated that using simple water as a solvent in the qNMR method is as effective as the HPLC method for the quantitative analysis of CIP. The investigated method accurately compensated for the deficiencies of the current HPLC method for quantitative measurement of CIP, and the use of PNP overcame the problem of absolute integration of signals associated with NMR spectra.</p>

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Ciprofloxacin Quantification with Nuclear Magnetic Resonance Spectroscopy in a Deuterium-Free Environment

  • Muhammad Azam,
  • Ataf Ali Altaf,
  • Muhammad Hamayun

摘要

The quantitative nuclear magnetic resonance (qNMR) method of quantifying the content of pharmaceuticals is an important and growing science in the current era. The deuterium-based solvents contribute to the main costs of the NMR-based analysis. In this study, we introduced the use of deuterium-free solvent (i.e., water H2O) for the quantification of ciprofloxacin (CIP) using the qNMR method. p-Nitrophenol (PNP) was used as an internal standard to solve the absolute integration of signals in NMR spectra. Quantification results were compared with literaturereported high-performance liquid chromatographic (HPLC) methods and analyzed by analysis of variance (ANOVA). The ANOVA results show that the regression model is highly significant (F = 37515.62, p < 0.001), indicating that the actual quantity of the analyte is a powerful predictor of the quantized concentration. An ANOVA study demonstrated that using simple water as a solvent in the qNMR method is as effective as the HPLC method for the quantitative analysis of CIP. The investigated method accurately compensated for the deficiencies of the current HPLC method for quantitative measurement of CIP, and the use of PNP overcame the problem of absolute integration of signals associated with NMR spectra.