Preconcentration and determination of chlordiazepoxide and diazepam drugs using dispersive nanomaterial-ultrasound assisted microextraction method followed by high performance liquid chromatography

J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Jan 1:1008:146-155. doi: 10.1016/j.jchromb.2015.11.043. Epub 2015 Nov 25.

Abstract

Benzodiazepines (BDs) are used widely in clinical practice, due to their multiple pharmacological functions. In this study a dispersive nanomaterial-ultrasound assisted- microextraction (DNUM) method followed by high performance liquid chromatography (HPLC) was used for the preconcentration and determination of chlordiazepoxide and diazepam drugs from urine and plasma samples. Various parameters such as amount of adsorbent (mg: ZnS-AC), pH and ionic strength of sample solution, vortex and ultrasonic time (min), and desorption volume (mL) were investigated by fractional factorial design (FFD) and central composite design (CCD). Regression models and desirability functions (DF) were applied to find the best experimental conditions for providing the maximum extraction recovery (ER). Under the optimal conditions a linear calibration curve were obtained in the range of 0.005-10μgmL(-1) and 0.006-10μgmL(-1) for chlordiazepoxide and diazepam, respectively. To demonstrate the analytical performance, figures of merits of the proposed method in urine and plasma spiked with chlordiazepoxide and diazepam were investigated. The limits of detection of chlordiazepoxide and diazepam in urine and plasma were ranged from 0.0012 to 0.0015μgmL(-1), respectively.

Keywords: Benzodiazepines; Central composite design; Dispersive nanomaterial-ultrasound assisted microextraction; Fractional factorial design; Plasma; Urine.

Publication types

  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Chlordiazepoxide / analysis*
  • Chlordiazepoxide / blood
  • Chlordiazepoxide / urine
  • Chromatography, High Pressure Liquid / methods*
  • Diazepam / analysis*
  • Diazepam / blood
  • Diazepam / urine
  • Humans
  • Microscopy, Electron, Transmission
  • Nanostructures*
  • X-Ray Diffraction

Substances

  • Chlordiazepoxide
  • Diazepam