Stability indicating RP-LC-PDA method for the quantitative analysis of saxagliptin in pharmaceutical dosage form

Abstract

Saxagliptin is a potent and selective inhibitor of the enzyme dipeptidyl peptidase 4. It is effective in the treatment of type 2 diabetes mellitus because it stimulates the pancreas to produce insulin. In the present study, a liquid chromatography method was developed and validated to quantify the drug in tablets. This method was based on the isocratic elution of saxagliptin, using a mobile phase consisting of 0.1% phosphoric acid at pH 3. 0 -methanol (70: 30, v/v) at a flow rate of 1 mL.min -1 with UV detection at 225 nm. The chromatographic separation was achieved in 8 minutes on a Waters XBridge C18 column (250 mm x 4.6 mm, 5µm) maintained at ambient temperature. The proposed method proved to be specific and robust for the quality control of saxagliptin in pharmaceutical dosage forms, showing good linearity in the range of 15.0 -100.0 µg.mL -1 (r>0.999), precision (RSD<1.49%) and accuracy values between 99.42 and 101.59%. The method was found to be stability indicating and was successfully applied for the analysis of saxagliptin in tablets in a routine quality control laboratory.Uniterms: Saxagliptin/tablets/quality control. High Performance Liquid Chromatography/quantitative analysis.A saxagliptina é uma inibidora potente e seletiva da enzima dipeptidil peptidase 4. É efetiva no tratamento do Diabete mellitus tipo 2, pois estimula a produção de insulina pelo pâncreas. No presente estudo, desenvolveu-se e validou-se método por cromatografia líquida de alta eficiência para quantificar o fármaco em comprimidos. O método foi baseado em eluição isocrática, utilizando fase móvel constituída por ácido fosfórico 0,1% pH 3,0-metanol (70 : 30, v/v), fluxo de 1,0 mL.min -1 , com detecção UV em 225 nm. A separação cromatográfica foi alcançada em 8 minutos em coluna Waters XBridge C18 (250 mm x 4,6 mm, 5 µm) mantida à temperatura ambiente. O método proposto mostrou-se específico e robusto para o controle de qualidade de saxagliptina em comprimidos, sendo linear na faixa de concentração de 15,0-100,0 µg.mL -1 (r>0,999), preciso (RSD<1,49%) e exato, com resultados entre 99,42 e 101,59%. O método mostrou-se indicativo de estabilidade e foi aplicado com sucesso no controle de qualidade de saxagliptina em comprimidos.Unitermos: Saxagliptina/comprimidos/controle de qualidade. Cromatografia líquida de alta eficiência/ análise quantitativa.

Application of quality by design approach in RP-HPLC method development for simultaneous estimation of saxagliptin and dapagliflozin in tablet dosage form

“…), is a potent, selective, long-acting, and reversible inhibitor of the enzyme dipeptidyl peptidase 4 (DPP-4) used for treatment of type 2 diabetes mellitus. It is used as monotherapy or in combination with other drugs (Scheeren et al, 2015;Hanan et al, 2017).…”

“…A few analytical methods were reported in the literature for the determination of SAXA alone. Stability indicating RP HPLC and RP-LC-PDA methods for determination of SAXA in pharmaceutical dosages were developed (Scheeren et al, 2015;Konari, Jacob, 2015). SAXA was estimated, with other antidiabetic drugs like vildagliptin, using spectrophotometric and spectrofluorimetric methods from bulk and pharmaceutical dosage forms (Marwa, 2013) and also with metformin hydrochloride, using the RP column liquid chromatographic method in binary mixtures (Mohammad, Ehab, Marwa, 2012), The HPLC method is used in active drug and pharmaceutical dosage forms (Hanan et al, 2017) and stability indicating RP HPLC method for the determination of saxagliptin and metformin in bulk and pharmaceutical product (Ramesh, Senthil Kumar, 2016).…”

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

“…Chemically, it is (1S,3S,5S)-2-((2S)-amino(3-hydroxytricyclo(3.3.1.13,7)dec-1yl)acetyl)-2-azabicyclo(3.1.0) hexane-3-carbonitrile ( Figure 1b) and has the molecular formula C 18 H 25 N 3 O 2 . [7][8][9] A review of the literature revealed that a few analytical methods like LC-Mass spectrometry, 10,11 HPLC, [12][13][14][15][16][17][18][19] and spectroscopic methods 20,21 are available for the estimation of these drugs, either individually or in combination with other diabetic drugs like metformin. [22][23][24][25][26] The present work aimed to develop a simple, rapid, and accurate method for the estimation of dapagliflozin and saxagliptin in human plasma, as per US-FDA guidelines.…”

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“…HPLC, LC-MS and, GC has been reported for estimation of Dapagliflozin and Saxagliptin individually or in combination with other drugs. The reported methods are Spectrophotometric [9][10][11][12][13][14][15] , HPLC [16][17][18][19][20][21][22][23][24][25][26][27][28][29][30][31][32][33][34][35] , LC-MS [36][37] and GC 38 method are reported for the simultaneous estimation of DAP and SAX in combined pharmaceutical formulation. Mobile Phase Preparation: Accurately weighed 2.72 g of Potassium dihydrogen phosphate transferred in a 1000 ml clean and dry volumetric flask, add about 900 ml of HPLC water and Sonicated for degassing and then finally make up the volume with water.…”