Malaysian Journal of Analytical Sciences Vol 25 No 1 (2021): 95 - 104

 

 

 

 

NOVEL AND VALIDATED NON-AQUEOUS TITRIMETRIC METHOD FOR DETERMINATION OF PERSPECTIVE POTASSIUM-SPARING DIURETIC DRUG CANDIDATE IN PURE FORM AND PHARMACEUTICAL FORMULATION

 

(Kaedah Titrimetrik Bukan Akues Novel dan Ditentusahkan bagi Penentuan Penahanan Kalium-Dadah Diuretik dalam Formulasi Tulen dan Farmaseutikal)

 

Alexey Ivanov¹*, Ivan Smırnov², Tatyana Murashko², Marina Trusova¹, Elena Stepanova¹

 

¹Research School of Chemistry & Applied Biomedical Sciences,

National Research Tomsk Polytechnic University, Tomsk, Russia

²The Faculty of Pharmacy,

Altai State Medical University, Barnaul, Russia

 

*Corresponding author: ivanovaa@tpu.ru

 

 

Received: 31 August 2020; Accepted: 22 November 2020; Published:  20 February 2021

 

 

Abstract

4-O-β-D-(glucopyranosyloxy)-benzoic acid sodium salt (4-GBA) is promising potassium-sparing diuretic and anti-inflammatory drug. For the survey of 4-GBA as pharmaceutical substance, a durable method of its quantification is needed. In the present study, a titrimetric method for 4-GBA quantification since it is evident, very simple, fast, applicable for routine analysis and there is no need of using reference standards was developed. Aqueous titration gave unsatisfactory result. Thus, based on the weak basic properties of the 4-GBA, non-aqueous titration was chosen. Glacial acetic acid was used as a solvent, and an anhydrous solution of perchloric acid in glacial acetic acid was used as a titrant. End-point detection was carried out potentiometrically (method A) and visually with violet crystalline as an indicator (method B). Using aqueous titration, we determined pK_a of 4-GBA as 4.27. The developed non-aqueous titration method is of excellent linearity (r² = 0.9995 and r² = 0.9947 for method A and method B, respectively), accuracy (recovery from 98.8 to 101.1 % and from 98.1 to 103.2 % for method A and method B, respectively) and precision (RSD ≤ 2% for intra- and inter-day analysis). The developed method is fast, simple, cheap and is applicable for the quantitative determination of 4-GBA both in pure form, bulk and pharmaceutical formulations.

 

Keywords:  glucosides, potassium-sparing diuretics, validation methods, non-aqueous titration, quantitative determination

 

Abstrak

Garam sodium 4-O-β-D-(glukopiranosiloksi)-asid benzoik (4-GBA) merupakan penahanan diuretik kalium dan dadah anti-radang yang berkesan. Dari tinjauan 4-GBA sebagai bahan farmaseutikal, satu kaedah tahan lasak bagi kuantifikasi adalah diperlukan. Dalam kajian ini, kaedah titrimetrik bagi kuantifikasi 4-GBA telah dibangunkan kerana ia terbukti ringkas, pantas dan aplikasi mudah bagi analisis rutin dan piawai rujukan tidak diperlukan. Pentitratan akues telah memberikan hasil yang tidak memuaskan. Maka berdasarkan sifat bes lemah 4-GBA, pentitratan bukan akues telah dipilih. Asid asetik glasier telah digunakan sebagai pelarut, dan larutan asid perklorik kontang di dalam asid asetik glasier telah digunakan sebagai titran. Pengesanan titik akhir telah dijalankan secara potentiometrik (kaedah A) dan secara visual dengan kehadiran hablur sebagai penunjuk (kaedah B). Berdasarkan pentitratan akues, nilai pKa 4-GBA ditentukan pada 4.27. Kaedah pentitratan bukan akues yang telah dibangunkan memberi nilai kelinearan baik (r² = 0.9995 dan r² = 0.9947 masing-masing bagi kaedah A dan B), ketepatan (perolehan semula dari 98.8 hingga 101.1% dan dari 98.1 hingga 103.2% masing-masing bagi kaedah A dan B) dan kejituan (RSD ≤ 2% bagi analisis intra dan inter-hari). Kaedah yang dibangunkan adalah pantas, mudah, murah dan kebolehgunaan bagi penentuan 4-GBA di dalam formulasi tulen, pukal dan farmaseutikal.

 

Kata kunci:  glukosida, penahanan diuretik kalium, kaedah tentusahkan, pentitratan bukan akues, penentuan kuantitatif

 

 

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