Analytical Control of Impurities and Active Ingredients in a (-)-Isopulegol Derivative with Highly Potent Analgesic Activity Full article
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Pharmaceutical Chemistry Journal
ISSN: 0091-150X , E-ISSN: 1573-9031 |
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| Output data | Year: 2020, Volume: 54, Number: 2, Pages: 190-194 Pages count : 5 DOI: 10.1007/s11094-020-02176-0 | ||||
| Tags | drug substance; (2R; 4R; 4aR; 7R; 8aR)-4; 7-dimethyl-2-(thiophen-2-yl)octahydro-2H-chromen-4-ol; HPLC-UV; validation | ||||
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Abstract:
An HPLC-UV procedure is proposed for identifying processing impurities and determining the contents of active ingredient in the drug substance of the promising non-narcotic analgesic (2R,4R,4aR,7R,8aR)- 4,7-dimethyl-2-(thiophen-2-yl)octahydro-2H-chromen-4-ol (1). Processing impurities including the starting reagents thiophene-2-carbaldehyde and (-)-isopulegol, a related stereoisomer of 1, and intermediates and dehydration products of 1 could be present as a result of the synthesis and isolation. The developed chromatography conditions could separate possible impurities and analyte 1 with the required resolution. The contents of the studied processing impurities were below the established detection limits of 0.056 mu g/mL for thiophene-2-carbaldehyde; 0.32, (-)-isopulegol; 0.22, the stereoisomer; and 0.18, 0.22, and 0.37, for the dehydration products. The working range of concentrations for the procedure was 0.50 - 10 mu g/mL. The recovery varied from 98.9 to 101.2% in the accuracy evaluation. The procedure was demonstrated to have sufficient accuracy. The average relative standard deviation in the intraday precision evaluation was 0.7%; in the interday precision assessment, 0.8%, which were below the acceptance criteria of 2.0 and 3.0%, respectively.
Cite:
Lastovka A.V.
, Fedeeva V.P.
, Il'ina I.V.
, Salakhutdinov N.F.
Analytical Control of Impurities and Active Ingredients in a (-)-Isopulegol Derivative with Highly Potent Analgesic Activity
Pharmaceutical Chemistry Journal. 2020. V.54. N2. P.190-194. DOI: 10.1007/s11094-020-02176-0 WOS Scopus РИНЦ OpenAlex
Analytical Control of Impurities and Active Ingredients in a (-)-Isopulegol Derivative with Highly Potent Analgesic Activity
Pharmaceutical Chemistry Journal. 2020. V.54. N2. P.190-194. DOI: 10.1007/s11094-020-02176-0 WOS Scopus РИНЦ OpenAlex
Original:
Ластовка А.В.
, Фадеева В.П.
, Ильина И.В.
, Салахутдинов Н.Ф.
АНАЛИТИЧЕСКИЙ КОНТРОЛЬ СУБСТАНЦИИ ПРОИЗВОДНОГО (-)-ИЗОПУЛЕГОЛА - СОЕДИНЕНИЯ С АНАЛЬГЕТИЧЕСКОЙ АКТИВНОСТЬЮ - ПО ПОКАЗАТЕЛЯМ "ТЕХНОЛОГИЧЕСКИЕ ПРИМЕСИ" И "ДЕЙСТВУЮЩЕЕ ВЕЩЕСТВО"
Химико-фармацевтический журнал (PHARM CHEM J+). 2020. Т.54. №2. С.43-48. DOI: 10.30906/0023-1134-2020-54-2-43-48 РИНЦ
АНАЛИТИЧЕСКИЙ КОНТРОЛЬ СУБСТАНЦИИ ПРОИЗВОДНОГО (-)-ИЗОПУЛЕГОЛА - СОЕДИНЕНИЯ С АНАЛЬГЕТИЧЕСКОЙ АКТИВНОСТЬЮ - ПО ПОКАЗАТЕЛЯМ "ТЕХНОЛОГИЧЕСКИЕ ПРИМЕСИ" И "ДЕЙСТВУЮЩЕЕ ВЕЩЕСТВО"
Химико-фармацевтический журнал (PHARM CHEM J+). 2020. Т.54. №2. С.43-48. DOI: 10.30906/0023-1134-2020-54-2-43-48 РИНЦ
Dates:
| Published print: | May 1, 2020 |
| Published online: | May 18, 2020 |
Identifiers:
| Web of science: | WOS:000533494400001 |
| Scopus: | 2-s2.0-85085180402 |
| Elibrary: | 43287040 |
| OpenAlex: | W3026902371 |