Short communication
Colourimetric and AAS determination of cephalosporins using Reineck's salt

https://doi.org/10.1016/S0731-7085(02)00040-7Get rights and content

Abstract

Two simple, accurate, sensitive and selective procedures for the determination of eight cephalosporins are described. These procedures are based on the formation of ion-pair complexes between the drugs and ammonium reineckate, the formed precipitates are quantitatively determined either colourimetrically or by atomic absorption spectrometrically. The methods consist of reacting drugs with Reinecke's salt in an acidic medium at 25±2°. The first colourimetric procedure (procedure I) is based on dissolving the formed precipitate with acetone, the volume was completed quantitatively and the absorbance of the solution was measured at 525 nm against pure solvent blank. Also, the formed precipitates on the atomic absorption spectrometric procedure (procedure II) are quantitatively determined directly or indirectly through the chromium precipitate formed or the residual unreacted chromium in the filtrate at 358.6 nm. The optimum conditions for precipitation have been carefully studied. Beer's law is obeyed for the studied drugs in the range 5–35 μg ml−1 with correlation coefficients ≮0.9989. Both procedures I and II hold well accuracy and precision when applied to the analysis of the cited cephalosporins in different dosage forms with good recovery percent ranged from 98.7±0.90 to 100.1±0.74 without interference from additives.

Introduction

Cephalosporins are penicillinase-resistant antibiotics with significant activity against Gram positive and Gram negative bacteria [1]. Cephalosporins were determined by titrimetric [2], [3], [4], [5], spectrophotometric [6], [7], [8], [9], [10], [11], [12], [13], [14], [15], [16], fluorimetric [17], [18], [19], [20], chromatographic [21], [22], [23], [24], [25], potentiometric [26] and polarographic [27], [28] methods.

Reineck's salt is ammonium tetrathiocyanotodiamminochromate (III) monohydrate in which it can be used for quantitative determination of many pharmaceutical compounds applying gravimetric [29], titrimetric [30] and spectrophotometric [31], [32], [33], [34], [35] procedures.

The purpose of the present work is to describe the development of the two simple and accurate spectrophotometric procedures, as well as a selective and sensitive atomic absorption spectrometric procedure, for the analysis of the titled antibiotic in the pure form as well as in pharmaceutical preparations.

Section snippets

Apparatus

  • A Shimadzu UV1601, UV-visible spectrophotometer (Tokyo, Japan).

  • A Shimadzu atomic absorption flame spectrophotometer model AA.640-13 with a chromium hollow cathode lamp under the following observation height above burner 1 cm; single slot type burner; air flow-rate 21.51/min; acetylene flow-rate 3.41/min operation conditions: lamp current 29 mA; slit width 0.7 nm; wavelength current 29 mA; slit width 0.7 nm; wavelength 358.6 nm.

Materials

All solvents and reagents were of analytical reagent grade.

Results and discussion

Mixing each aqueous solution of cephaprin sodium, cefuroxime sodium, cefotaxime sodium, cefoperazone sodium, cefadroxil, ceftazidime, cefazolin sodium or cefaclor with ammonium reineckate in acidic medium at 25±2 °C resulted in the formation of red precipitate. It is based on the formation of ion-pair complexes between the drugs and ammonium reineckate.

Formation of drug-reineckate ion-pair complexes allows indirect determination of these drug by atomic absorption spectrometric measurement of the

References (37)

  • V. Rodenas et al.

    J. Pharm. Biomed. Anal.

    (1997)
  • L. Gallo-Martinez et al.

    J. Chromatogr. Biomed. Appl.

    (1998)
  • M.M. Ayad et al.

    J. Pharm. Biomed. Appl.

    (1999)
  • M.M. Ayad et al.

    J. Pharm. Biomed. Appl.

    (1999)
  • A. Kar et al.

    J. Pharm. Sci.

    (1981)
  • Wilson and Gisfold's Text Book of Organic Medicinal and Pharmaceutical Chemistry, tenth ed., J.B. Lippincott, Raven,...
  • J.R. Grime et al.

    Anal. Chim. Acta

    (1979)
  • A.G. Fogg et al.

    Analyst

    (1982)
  • B. Pospisilova et al.

    Pharmazie

    (1988)
  • S.A. Nabi et al.

    Chem. Anal.

    (1997)
  • J.A. Murillo et al.

    Anal. Lett.

    (1994)
  • M.I. Walash et al.

    Anal. Lett.

    (1994)
  • A. Dimitrovska et al.

    Anal. Lett.

    (1996)
  • Y.M. Issa et al.

    Mikrochim. Acta

    (1996)
  • D. Agaba et al.

    Spec. Lett.

    (1997)
  • K. Kelani et al.

    J. Assoc. Off. Anal. Chem.

    (1998)
  • A.B. Avadhanlu et al.

    Indian Drugs

    (1999)
  • M.D. Blanchin et al.

    Analyst

    (1985)
  • Cited by (57)

    • Adsorption behavior of hydroxypropyl guar gum onto montmorillonite and reducing adsorption in the reservoir

      2018, Applied Clay Science
      Citation Excerpt :

      So far the most popular used fracturing fluids in oil field are emulsion polymers (Ianchis et al., 2009), viscoelastic surfactant (VES) (Hull et al., 2015; Li et al., 2016) and modified guar gum. The concentration of emulsion polymer and VES would be determined through using starch‑cadmium iodide method and reinecke salt colorimetric method, respectively (Scoggins and Miller, 1979; Salem and Askal, 2002). In previous work (Yin et al., 2018), the determination method of cellulose was referred to measure the concentration of HPG, and the similar method was also used in this paper.

    • The adsorption behavior of hydroxypropyl guar gum onto quartz sand

      2018, Journal of Molecular Liquids
      Citation Excerpt :

      Currently, the commonly used fracturing fluids in oilfields are based on modified guar gum, emulsion polymer [11,12] and viscoelastic surfactant (VES) [13,14]. The concentration of VES and emulsion polymer could be measured with the colorimetric method using the Reinecke salt and the starch‑cadmium iodide method, respectively [15–17]. However, the adsorption of HPG (the most commonly used thickener in fracturing fluids) on the reservoir rocks has not been fully studied.

    • Mechanistic investigation of the oxidation of Cefuroxime by hexacyanoferrate(III) in alkaline conditions

      2013, Journal of Industrial and Engineering Chemistry
      Citation Excerpt :

      Several methods have been reported, for the analysis of CFA in pharmaceutical and physicochemical preparation. It has also been assayed spectrofluorimetrically [5,6], colourimetric and atomic absortion spectrophotometry based upon the complexation with Reinecke's salt [7]. Atomic absorption procedure based on the reaction with silver nitrate/lead acetate at pH 7 [8] and, spectrophotometric methods after complexation with 7,7,8,8-tetracyanoquinodimethane, p-chloranilic acid, Prussian Blue and reaction with metol-chromium (VI) reagent [9,10] have been explored.

    View all citing articles on Scopus
    View full text