A simple method for the quantification of diclofenac potassium in oral suspension by high-performance liquid chromatography with UV-detection

Abstract

A rapid, simple and low cost method was developed to determine diclofenac potassium (DP) in oral suspension, using a reverse-phase column (C 8 , 150 mm x 4.6 mm, 5 µm), mobile phase containing methanol/buffer phosphate (70:30 v/v, pH 2.5), at a flow rate of 1.0 mL/min, isocratic method, and ultraviolet detection at 275 nm. A linear response (r = 1.0000) was observed in the range of 10.0-50.0 µg/ mL. Validation parameters such as linearity, specificity, precision, accuracy and robustness were evaluated. The method presented precision (repeatability: relative standard deviation = 1.21% and intermediate precision: between-analyst = 0.85%). The specificity of the assay was evaluated by exposure of diclofenac potassium under conditions of stress such as hydrolysis, photolysis, oxidation and high temperature. The method presented accuracy values between 98.28% and 101.95%. The results demonstrate the validity of the proposed method that allows determination of diclofenac potassium in oral suspension and may be used as an alternative method for routine analysis of this product in quality control.Uniterms: High performance liquid chromatography. Diclofenac potassium. Oral suspension.Desenvolveu-se método simples, de baixo custo para determinar o diclofenaco potássico (DP) em suspensão oral, usando coluna de fase reversa (C 8 , 150 mm x 4,6 mm, 5 µm), fase móvel contendo metanol/tampão fosfato (70:30 v/v, pH 2,5), com fluxo de 1,0 mL/min, método isocrático e detecção no ultravioleta a 275 nm. Observou-se resposta linear (r = 1,0000) na faixa de 10,0-50,0 µg/mL. Avaliaramse parâmetros de validação, como linearidade, especificidade, precisão, exatidão e robustez. O método apresentou precisão (repetibilidade: desvio padrão relativo = 1,21% e precisão intermediária: entre analista = 0,85%). A especificidade do ensaio foi avaliada pela exposição do diclofenaco potássico a condições de estresse, tais como hidrólise, fotólise, oxidação e alta temperatura. O método apresentou valores de exatidão entre 98,28% e 101,95%. Os resultados mostram a validade do método proposto, que permite a determinação de diclofenaco potássico em suspensão oral e pode ser utilizado como alternativa para análise de rotina desse produto no controle de qualidade. Unitermos: Cromatografia de alta eficiência. Diclofenaco potássico. Suspensão oral.

Application of Thin-Layer Chromatography in Combination with Densitometry for the Determination of Diclofenac in Enteric Coated Tablets

“…The low coefficient of variation values (CV < 3%) was indicative of the accuracy of the method. Moreover, the obtained accuracy was comparable to the mean results of accuracy of HPLC method developed for the determination of diclofenac potassium in oral suspension (RSD% = 98.28-101.95) and better in relation to accuracy of HPLC procedure described for analysis of diclofenac sodium in form of commercial tablets [44]. The mean percentage of recovery of examined active ingredient in tablets was 95.2 ± 4.9% [45].…”

“…According to American Pharmacopeia the content of diclofenac sodium in tablets should be in the range 90-110% [36]. The results obtained by means of proposed TLC-densitometric method were comparable with diclofenac content determined with the use of HPLC procedures in oral suspension and tablets [44,45]. This proved that the proposed method was an alternative for the determination of diclofenac in enteric coated tablets.…”

“…Since CV values for repeatability and intermediate were <3% the method was precise. In the case of HPLC method dedicated for the analysis of examined drug substance in oral suspension, the repeatability and intermediate precision expressed as relative standard deviation was 1.21% and 0.85%, respectively [44]. Thus, it was less than 2%.…”

Simultaneous Electrochemical Determination of Paracetamol and Diclofenac Based on Poly(diallyldimethylammonium chloride) Functionalized Graphene

“…Diclofenac (DCF) is an acid phenyl acetic derivative with anti‐inflammatory, analgesic and anti‐thermal properties. The drug is indicated for rheumatoid arthritis, degenerative joint disease, chronic pain associated with cancer and kidney stones and endodontic procedures 1, 2. DCF has been found to increase the blood pressure in patients with Shy‐Drager syndrome and diabetes mellitus and could also cause life‐threatening heart or circulation problems such as heart attack and stroke especially when used by patients for a long time 3.…”

Quality by Design Determination of Diclofenac Potassium and its Impurities by High-Performance Liquid Chromatography

“…Many reports have described LC methods for the determination of diclofenac sodium or diclofenac potassium and other drugs in pharmaceutical formulations (Ye and Zhang 2000;Krzek and Starek 2002;Bisas and Basu 2010;Elkady 2010;Gowramma et al 2010;Khatal et al 2010;Rele et al 2011;Ambekar, Choudhari, and Ingale 2012;Chaple et al 2012;Panda, Patanaik, and Ravi Kumar 2012;Rubim et al 2013;Shaalan and Belal 2013;Belal et al 2014;Rubim et al 2014). Here these impurities were investigated together for the first time.…”