Highly sensitive luminescence determination of flupirtine maleate
Identification of the active pharmaceutical ingredients in washings from surfaces of pharmaceutical equipment is necessary to avoid cross-contamination of the next batch of products. The aim of this work – the development of the method of luminescence determination of residual active pharmaceutical ingredients flupirtine maleate in washings to monitor the completeness of its removal for cleaning technologic equipment.
In this work the flupirtine maleate substance and 0.1 M hydrochloric acid were used. The excitation spectra and luminescence spectra were recorded on a spectrofluorimeter Cary Eclipse «Varian». Electronic absorption spectra were recorded on a spectrophotometer UV-2401 PC «Shimadzu».
The absorption spectrum of an flupirtine maleate in 0.1 M hydrochloric acid solution characterized by intense bands in the UV region of the spectrum with maxima at λ = 246 nm and λ = 345 nm. Luminescence excitation spectrum of the flupirtine maleate solution almost the same as its absorption spectrum.
The ionization constants of flupirtine maleate by the standard spectrophotometric and fluorescent methods were determined. pK values of flupirtine maleate were calculated in the program Origin 7.5, are 5.45 ± 0.02 and 5.71 ± 0.03, respectively, and indicate satisfactory correlation results obtained by the two different methods.
The recovery rates of flupirtine maleate from swabs was more than 95%.
The highly sensitive, simple and rapid method for determination of flupirtine maleate by its own luminescence in the 0.1 M solution of hydrochloric acid (λex = 345 nm; λlum = 427 nm) in washings from surfaces of pharmaceutical equipment was developed. Calibration curve was linear over the concentration range of the flupirtine maleate 0.01–0.5 µg/ml. The limit of detection is 0.003 µg/ml.
The developed method can be recommended for the determination of residual amounts of flupirtine maleate in the quality control of pharmaceutical equipment cleaning.
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