DEVELOPMENT OF A QUANTITATIVE DETERMINATION METHODOLOGY FOR THE CERTIFICATION OF THE PRIMARY STANDARD SAMPLE OF A NEW ANALGESIC AGENT – 1-(PHENYL[PHENYLIMINO]METHYL)PYRROLIDINE-2,5-DIONE
Abstract
Aim. The article presents an approach to the development of a quantitative determination technique for the certification of the primary standard sample of a new analgesic agent ‒ 1-(phenyl[phenylimino]methyl)pyrrolidine-2,5-dione (PPMP) by titration using the Kjeldahl method. Due to the non-specificity of this method and the high probability of the presence of nitrogen-containing impurities in the substance certified, it was proposed to purify the substance certified to the maximum possible degree of purity. To confirm the purity of the substance, a method of analysis for the indicator "Limit content of related impurities" with high performance liquid chromatography (HPLC) method was developed and validated.
Material and methods. Chromatographic separation in acetonitrile / 0.15% aqueous formic acid solution (pH 2.5) phases in gradient mode on a Tosoh ODS column (4.6×250 mm, 5 microns) with a flow rate of 1.0 ml/min was achieved in 35 minutes. The signal was recorded using a multi-wave UV detector at a wavelength of 257 nm.
Conclusions. Using a validated technique, it was proved that the purity of the substance is 100.0%. According to the Kjeldahl method, a quantitative assessment of the content of the main substance in the purified FFMP substance was carried out, its certified value was 99.7 ± 0.2%.
About the Authors
Yu. A. Trukhanova
ФГБОУ ВО «Санкт-Петербургский государственный химико-фармацевтический университет» Минздрава России
Russian Federation
Russian Federation
G. M. Alekseeva
ФГБОУ ВО «Санкт-Петербургский государственный химико-фармацевтический университет» Минздрава России
Russian Federation
Russian Federation
I. P. Yakovlev
ФГБОУ ВО «Санкт-Петербургский государственный химико-фармацевтический университет» Минздрава России
Russian Federation
Russian Federation
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Review
For citations:
Trukhanova Yu.A., Alekseeva G.M., Yakovlev I.P. DEVELOPMENT OF A QUANTITATIVE DETERMINATION METHODOLOGY FOR THE CERTIFICATION OF THE PRIMARY STANDARD SAMPLE OF A NEW ANALGESIC AGENT – 1-(PHENYL[PHENYLIMINO]METHYL)PYRROLIDINE-2,5-DIONE. Bashkortostan Medical Journal. 2022;17(6):41-45. (In Russ.)
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