Simultaneous Estimation of Saxagliptin and Dapagliflozin in Human Plasma by Validated High Performance Liquid Chromatography - Ultraviolet Method

Abstract

Saksagliptin ve dapagliflozinin sabit doz kombinasyonu antidiyabetik ilaç tedavisi için onaylanmıştır ve Qtern markası ile pazarda yer almaktadır. Bu çalışmada amaç, insan plazmasındaki saksagliptin ve dapagliflozinin eş zamanlı tayini için Avrupa Gıda ve İlaç İdaresi kılavuzlarına uygun şekilde linagliptin iç standardı kullanarak ve basit, hızlı, hassas ve validasyonu yapılmış izokroatik ters faz-yüksek performanslı sıvı kromatografi (RP-HPLC) yöntemi geliştirmektir. Gereç ve Yöntemler: Method 4'lü akış pompasına sahip Waters 2695 marka HPLC cihazı ile gerçekleştirilmiştir. Analitin ayrılmasında Eclipse XDB C18 kolon (150 × 4.6 mm × 5 μm) kullanılmıştır. Kullanılan mobil fazın bileşimi ise pH 5.0 ayarlanmış %0.1 orto fosforik asit ve asetonitril (50:50) şeklinde olup akış hızı analiz süresince 1 mL/dk'dır. Bulgular: Analit 254 nm'de tayin edilmiştir. İç standart, saksagliptin ve dapagliflozinin alıkonma zamanları sırasıyla 2.746, 5.173 ve 7.218 dk olarak tespit edilmiştir. Pikler interferanslar gözlenmeden elde edilmiştir. Metot validasyonu saksagliptin ve dapagliflozin için sırasıyla 0.01 ile 0.5 μg/mL ve 0.05 ile 2 μg/mL doğrusal derişim aralığında 0.998 korelasyon katsayısı ile gerçekleştirilmiştir. Numunlere ait 6 ölçüme ait kesinlik ve doğruluk tayin sınırları içerisinde bulunmuştur. Analitlerin insan plazması içinde-28°C sıcaklıkta 37 gün boyunca kararlı halde kaldığı belirlenmiştir.

Multivariate optimization of liquid chromatographic conditions for determination of dapagliflozin and saxagliptin, application to an in vitro dissolution and stability studies

“…Present method was found to be cost-effective owing to utilization of low % (26%) organic mobile phase than latest literature [10]. The analytical run duration for the proposed method is short (6 min); hence, this method was rapid and superior than literature methods [8,[11][12][13].…”

“…Literature survey revealed that there were few reports published on the simultaneous quantification of dapagliflozin and saxagliptin using UV [8], HPTLC [9], HPLC [10][11][12][13][14][15][16][17][18], and LC-MS [19,20] techniques in bulk drug and pharmaceutical dosage forms. Few methods were reported for analysis of dapagliflozin and saxagliptin separately [21][22][23][24] and in combination with other drugs [25][26][27][28][29].…”

A Stability Indicating RP-HPLC Method Validation for Simultaneous Estimation of Metformin HCl, Dapagliflozin and Saxagliptin in Pharmaceutical Dosage Form

“…3 respectively: [12][13][14]. After reviewing the literature, it can be said that individual analytical methods [15][16][17][18][19][20][21][22][23][24] are available for Metformin HCl, Dapagliflozin and Saxagliptin however, no RP-HPLC method is available for simultaneous estimation of Metformin HCL, Dapagliflozin and Saxagliptin in pharmaceutical dosage from as FDC. Developing Stability indicating RP-HPLC method for simultaneous estimation of Metformin HCl, Dapagliflozin and Saxagliptin in pharmaceutical dosage from as FDC is both requirement and challenge.…”

Second‐derivative synchronous spectrofluorimetric assay of dapagliflozin: Application to stability study and pharmaceutical preparation

“…) that acts as a sodium inhibitor of glucose co‐transporters Based on a survey of the published literature (Supporting Information Tables S1 and S2), some methods described DGF quantification either in its pure form or in its tablet dosage form for use in assays and/or stability studies. These methods included spectrophotometric and chromatographic methods , but suffered from either low sensitivity or difficulty, or high cost of analysis. A new simple, cheap and sensitive method is therefore urgently needed for analysis of DGF in both bulk and its commercially dosage forms to establish as a quality control.…”

“…These methods included spectrophotometric and chromatographic methods [5][6][7][8][9][10][11][12][13][14][15][16][17][18][19][20][21][22] , but suffered from either low sensitivity or difficulty, or high cost of analysis. A new simple, cheap and sensitive method is therefore urgently needed for analysis of DGF in both bulk and its commercially dosage forms to establish as a quality control.…”