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Development and validation of a new RP-HPLC-UV method for the simultaneous determination of phenytoin impurities, benzophenone, and benzil

Sungthong Bunleu, Rattarom Ruchilak, Sato Vilasinee Hirunpanich, Sato Hitoshi

Acta Chromatographica

2019

Vol. 31, no. 4

241--245

A new reversed-phase high-performance liquid chromatographic method with ultraviolet detection (RP-HPLC-UV) for simultaneous determination of phenytoin impurities, benzophenone and benzil, was developed and validated according to the International Council for Harmonization (ICH) guidelines. Chromatographic separation was performed on a C8 column using acetonitrile–1% acetic acid (60:40, v/v). The correlation coefficients of the calibration lines were greater than 0.999 with 95% confident interval of y-intercept over the origin. The analytical method showed good precision, intra-day precision ≤1.00 and inter-day precision ≤1.53. The standard solution of each compound exhibited good stability 99.18–99.70%, after storage at room temperature for 24 h. The limit of detection (LOD) and limit of quantification (LOQ) were 0.0015 and 0.005 μg/mL, respectively. The resolution of the impurities was 2.935 ± 0.009. The proposed analytical method was successfully applied to determine the amount of benzophenone and benzil in marketed products. The amount of benzophenone was found at 3.09–5.91 × 10−3%, while benzil was not detected in the samples.

Synthesis, Structural Characterization, Redox and Antimicrobial Studies of Schiff Base Copper(II), Nickel(II), Cobalt(II), Manganese(ii), Zinc(II) and Oxovanadium(ii) Complexes derived from benzil and 2-Aminobenzyl Alcohol

Raman N., Kulandaisamy A., Jeyasubramanian K.

Polish Journal of Chemistry

2002

Vol. 76 / nr 8

1085-1094

Neutral complexes of Cu(II), Ni(II), Co(II), Mn(II), VO(II) and Zn(II) have been synthesized from the Schiff base derived from benzil and 2-aminobenzyl alcohol. The structural features have been arrived from their microanalytical, IR, UV-Vis, 1H NMR, Mass and ESR spectral data. All of the complexes exhibit square-planar geometry except the Mn(II) and VO(II) complexes. The Mn(II) chelate shows an octahedral environment and the VO(II) chelate exists in a square-pyramidal geometry. The monomeric and non-electrolytic nature of the complexes is evidenced by their magnetic susceptibility and low conductance data. The cyclic voltammogram of copper complex in acetonitrile solution shows two quasi reversible peaks for the Cu(II)/Cu(III) and Cu(II)/Cu(I) couples. The X-band ESR spectra of the Cu(II) and VO(II) complexes in DMSO at 300 and 77 K were recorded and their salient features are reported. The biological activity of the metal chelates against the bacteria Staphylococcus aureus, Bacillus subtilis, Klebsiella pneumoniae, Salmonella typhi, Pseudomonas aeruginosa and Shigella flexneri are also reported. Most of the complexes have higher activity than that of the free Schiff base and the control.