Quantitative1H NMR spectroscopic determination of theE/Z isomer ratio of the antidepressant drug fluvoxamine for use in pharmaceutical analysis

In this study, two simple and accurate spectrophotometric methods were presented for the determination of duloxetine hydrochloride (DLX) in pharmaceutical preparations. The methods were based on the reaction of DLX asn-electron donor with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) and 7,7,8,8-tetracyanoquinodimethane (TCNQ) as π-acceptors to give highly colored complex species. The colored products were quantitated spectro-photometrically at 477 and 841 for DDQ, TCNQ, respectively. All variables were studied in order to optimize the reaction conditions. Beer's law was obeyed in the concentration ranges 10.0-50.0 and 15-60 μg mL−1for DDQ and TCNQ method, respectively. The proposed methods have been successfully applied to the pharmaceutical analysis without any interference from excipients. The suggested procedures could be used for the determination of DLX in pharmaceutical preparations being sensitive, simple and selective.

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Conventional and Microwave Prompted Synthesis of Aryl(alkyl)azole Oximes, 1H-NMR Spectroscopic Determination of E/Z Isomer Ratio and HOMO-LUMO Analysis

Journal of Molecular Structure ◽

10.1016/j.molstruc.2021.132077 ◽

2021 ◽

pp. 132077

Author(s):

İrem BOZBEY ◽

Harun USLU ◽

Burçin TÜRKMENOĞLU ◽

Zeynep ÖZDEMİR ◽

Arzu KARAKURT ◽

...

Keyword(s):

1H Nmr ◽

Spectroscopic Determination ◽

Isomer Ratio ◽

Homo Lumo

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Recent Applications of High Performance Thin Layer Chromatography and Derivative Spectrophotometry in Pharmaceutical Analysis

Current Pharmaceutical Analysis ◽

10.2174/1573412915666190226155149 ◽

2020 ◽

Vol 16 (6) ◽

pp. 671-689

Author(s):

Marcin Gackowski ◽

Marcin Koba ◽

Katarzyna Mądra-Gackowska ◽

Piotr Kośliński ◽

Stefan Kruszewski

Keyword(s):

Thin Layer ◽

Thin Layer Chromatography ◽

Pharmaceutical Analysis ◽

High Performance ◽

Degradation Products ◽

Derivative Spectrophotometry ◽

Accuracy And Precision ◽

Post Marketing ◽

Layer Chromatography

At present, no one can imagine drug development, marketing and post-marketing without rigorous quality control at each stage. Only modern, selective, accurate and precise analytical methods for determination of active compounds, their degradation products and stability studies are able to assure the appropriate amount and purity of drugs administered every day to millions of patients all over the world. For routine control of drugs simple, economic, rapid and reliable methods are desirable. The major focus of current scrutiny is placed on high-performance thin layer chromatography and derivative spectrophotometry methods, which fulfill routine drug estimation’s expectations [1-4]. The present paper reveals state-of-the-art and possible applications of those methods in pharmaceutical analysis between 2010 and 2018. The review shows advantages of high-performance thin layer chromatography and derivative spectrophotometry, including accuracy and precision comparable to more expensive and time-consuming methods as well as additional fields of possible applications, which contribute to resolving many analytical problems in everyday laboratory practice.

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