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The combination of Dipyridamole and Aspirin and is widely used to reduce thrombosis in patients with thrombotic diseases. A rapid, simple, precise and cost effective and reversed-phase high performance liquid chromatography (RP-HPLC) method has been developed and validated for the simultaneous determination of Aspirin and Dipyridamole in pharmaceut...
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Studies have shown aspirin decreases the risk of some cancers. However, the evidence reported the association between aspirin and cancer risk in the diabetic population. In this study, we investigate whether aspirin and dipyridamole decrease the risk of cancer in patients with type 2 diabetes. A total of 5308 patients with type 2 diabetes were iden...
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... The flow rate was 1.0 mL/min. Detection was performed at 227 nm; the injection volume was 100 µL [88,89]. ...
... Calibration Curve. References [88,91,115] ...
Citation: Maded, Z.K.; Sfar, S.; Taqa, G.A.A.; Lassoued, M.A.; Ben Hadj Ayed, O.; Fawzi, H.A. Development and Optimization of Dipyridamole-and Roflumilast-Loaded Nanoemulsion and Nanoemulgel for Enhanced Skin Permeation: Formulation, Characterization, and In Vitro Assessment. Pharmaceuticals 2024, 17, 803. https://doi. Abstract: This study explores developing and optimizing a nanoemulsion (NE) system loaded with dipyridamole and roflumilast, aiming to improve skin penetration and retention. The NE formulation was further transformed into a nanoemulgel to enhance its application as a topical treatment for psoriasis. Solubility studies were conducted to select the oil, surfactant, and co-surfactant. Phase diagrams were constructed using the aqueous phase titration method. All the formulations were in nanoscale, and Formula (F2) (which contains oleic acid oil as the oil phase, a mixture of Surfactant Tween 80 and co-surfactant (ethanol) at a ratio of 1:2 in addition to distilled water as an aqueous phase in a ratio of 1:5:4, respectively) was the selected formula depending on the particle size, PDI, and zeta potential. Formula (F2) has the best ratio because it gives the smallest nanoemulsion globule size (particle size average of 167.1 nm), the best homogenicity (lowest PDI of 0.195), and the highest stability (higher zeta potential of −32.22). The selected formula was converted into a nanoemulgel by the addition of 0.5% (w/w) xanthan gum (average particle size of 172.7 nm) and the best homogenicity (lowest PDI of 0.121%) and highest stability (higher zeta potential of −28.31). In conclusion, the selected formula has accepted physical and chemical properties, which enhanced skin penetration.
... Aspirin had been analyzed either in single formulation or in multi-component medications using UV-VIS spectrophotometry [11][12][13][14][15][16], chromatography; HPLC [17][18][19][20][21][22][23][24], UPLC [25] and TLC methods [26,27] and electrochemical analysis [28,29]. While, for rivaroxaban, the literature shows determination of ROX by spectrophotometric methods [30,31] and many chromatographic methods for quantification of ROX in its dosage form via HPTLC [32,33], HPLC [34][35][36] and in plasma [37,38]. ...
Patients diagnosed with symptomatic peripheral artery disease (PAD) in the lower extremities have a higher likelihood of suffering from major vascular events. Recently, FDA has approved the combination therapy of aspirin (ASP) and rivaroxaban (ROX) to reduce acute limb ischemia and other comorbidities in (PAD) patients. Zero order and ratio absorption spectra were employed in three simple and accurate spectrophotometric techniques (dual wavelength (DW), ratio difference (RD) and derivative ratio (¹DD) for concurrent detection and quantification of ASP and ROX in their pure forms, lab synthetic mixtures and in biological fluid. Our approach involves careful parameter optimization, including solvent selection, sample volumes, and instrumental settings, to reduce the analysis environmental impact. The acquired recovery percentages of accuracy were within 98–102% for pure active pharmaceutical ingredients and 90–110% for pharmaceutical formulations and biological determinations. A comprehensive assessment was done to compare the three methods regarding their ease of use, linearity, sensitivity, conditions, and limitations. The specificity of the proposed methods was evaluated by analyzing the lab synthetic mixtures. The suggested spectrophotometric methods were validated in compliance with ICH guidelines to confirm the validity claims. Also, statistical analysis was done to compare the outcomes obtained from the suggested methods with those obtained from the official ones and they agreed with null hypothesis regarding accuracy and precision. Furthermore, a comprehensive assessment of the environmental sustainability of the developed method was carried out using the Analytical Greenness Calculator, AGREE algorithm. The selected drugs can be efficiently, safely and economically analyzed by the suggested methods in pharmaceutical and biological matrices with no pretreatment or preliminary separation steps and thereby increasing their greenness level.
... Overall, due to its impressive benefits, DIP determination in pharmaceuticals and various biological samples became really important. There are numerous analytical methods proposed for this drug quantification which encompass more conventional techniques, such as HPLC [6][7][8][9][10] and spectrophotometry [11,12]. Despite their advantages, these methods have also shown important limitations, such as the need for time-consuming preliminary procedures, such as extraction and concentration in organic solvents, that imply large volumes of samples and reagents, expensive equipment, and the necessity of specialized personnel, in the case of chromatographic methods. ...
... The electroactive areas of the bare PGE, NIP_PGE, and MIP_PGE were assessed by performing cyclic voltammetry recordings at various scan rates at each of the listed working electrodes in 1.00 × 10 −4 mol/L K 4 Fe(CN) 6 in 0.10 mol/L KCl solution and using the slopes of the regression equations of the I p (A) = f(v 1/2 , (V/s) 1/2 ) dependencies and the Randles-Sevcik equation I p (A) = 2.95 × 10 5 × n 3/2 × A ea × D 1/2 × C 0 × v 1/2 , where I p (A) is the peak current; n is the number of transferred electrons(n = 1); A ea (cm 2 ) is the electrode electroactive surface area; D (cm 2 /s) is the diffusion coefficient of K 4 Fe(CN) 6 in 0.1 mol/L KCl (D = 7.6 × 10 −6 cm 2 /s) [28]; v (V/s) is the scan rate, and C 0 (mol/cm 3 ) is the concentration of K 4 Fe(CN) 6 . ...
... The electroactive areas of the bare PGE, NIP_PGE, and MIP_PGE were assessed by performing cyclic voltammetry recordings at various scan rates at each of the listed working electrodes in 1.00 × 10 −4 mol/L K 4 Fe(CN) 6 in 0.10 mol/L KCl solution and using the slopes of the regression equations of the I p (A) = f(v 1/2 , (V/s) 1/2 ) dependencies and the Randles-Sevcik equation I p (A) = 2.95 × 10 5 × n 3/2 × A ea × D 1/2 × C 0 × v 1/2 , where I p (A) is the peak current; n is the number of transferred electrons(n = 1); A ea (cm 2 ) is the electrode electroactive surface area; D (cm 2 /s) is the diffusion coefficient of K 4 Fe(CN) 6 in 0.1 mol/L KCl (D = 7.6 × 10 −6 cm 2 /s) [28]; v (V/s) is the scan rate, and C 0 (mol/cm 3 ) is the concentration of K 4 Fe(CN) 6 . ...
A new method for the determination of the antiplatelet drug dipyridamole (DIP) in pharmaceuticals using a molecularly imprinted polymer (MIP)-modified pencil graphite electrode (PGE) is proposed. The modified electrode was prepared simply and rapidly by electropolymerization of caffeic acid (CA) in the presence of DIP and subsequent DIP extraction with ethanol, resulting in a cost-effective, eco-friendly disposable modified electrode (MIP_PGE). Several working conditions (monomer and template concentration, number of voltametric cycles, scan rate extraction time, and solvent) for the MIP_PGE preparation were optimized. The differential pulse voltammetric (DPV) oxidation signal of DIP obtained at MIP_PGE was 28% higher than that recorded at bare PGE. Cyclic voltammetry emphasized DIP irreversible, pH-dependent, diffusion-controlled oxidation at MIP_PGE. Differential pulse and adsorptive stripping voltammetry at MIP_PGE in phosphate buffer solution pH = 7.00 were applied for the drug quantitative determination in the range of 1.00 × 10−7–1.00 × 10−5 and 1.00 × 10−8–5.00 × 10−7 mol/L DIP, respectively. The obtained limits of detection were at the tens nanomolar level.
... A literature survey indicated that various chromatographic methods have been utilized for the estimation of DIP in pharmaceutical preparations (Bridle & Brimble, 1993;Zhang, Miller, & Jacobus, 1997;Zoesta et al., 1991). While most studies estimated DIP in a mixture with other drug combinations, only few specifically estimated DIP and its degradation product (Hassan et al., 2008;Prakash, Rama Rao, & Jayapal Reddy, 2011;Rajput & Sonanis, 2011). ...
The current study was developed and validated for determination of dipyridamole related impurities in the pharmaceutical dosage forms using RP‐HPLC technique. The separation of all impurities were achieved with a YMC pack C8, (150 mm × 4.6 mm, 3.0 μm) analytical column and a suitable mobile phase. The mobile phase ‐ A contains 10mM concentration of phosphate buffer (adjusted to 4.7 by diluted orthophosphoric acid) and mobile phase ‐ B contains buffer: acetonitrile: methanol in the ratio of 30:40:30 v/v respectively. The optimized chromatographic conditions such as flow rate 1.0 ml/min, the detection was carried out at 295 nm, injection volume 10μl and the column temperature 35°C. The stressed samples were analyzed for the degradation study in acid, base, peroxide, water hydrolysis, and physical degradation studies. The proposed method was validated as per ICH guideline, and found to be specific, linear, accurate, robust stability‐indicating nature. The described method showed excellent linearity over a range of LOQ to 150% level of concentrations for all impurities. The correlation coefficient (r2) value achieved all impurities between 0.995 to 0.999, respectively. The recovery study was established from LOQ to 150% level concentrations. The mean recovery values were achieved between 92.9 to 103.2%, respectively. The current method can be used to determine the dipyridamole and it’s relative impurities. Based on the degradation and validated results, it’s a stability‐indicating nature. So, this method could be used in pharmaceutical R&D and QC departments.
... In the literature survey, quite a few GC method have been reported from the determination of the residual solvents in dipyridamole API [4], few liquid chromatographic methods have been reported for determination of dipyridamole in pharmaceutical preparation [4][5][6], and few methods have been reported for dipyridamole and its degradation product [7,8]. However, several methods were reported for determination of dipyridamole in combination with other drugs [9][10][11][12]. Estimation of dipyridamole and its metabolites in human plasma by liquid chromatographicmass spectroscopy and HPLC has been performed [13][14][15]. ...
A simple, sensitive, accurate, robust headspace gas chromatographic method was developed for the quantitative determination of acetone and isopropyl alcohol in tartaric acid-based pellets of dipyridamole modiied release capsules. e residual solvents acetone and isopropyl alcohol were used in the manufacturing process of the tartaric acid-based pellets of dipyridamole modiied release capsules by considering the solubility of the dipyridamole and excipients in the diierent manufacturing stages. e method was developed and optimized by using fused silica DB-624 (30 m × 0.32 mm × 1.8 µm) column with the ame ionization detector. e method validation was carried out with regard to the guidelines for validation of analytical procedures Q2 demanded by the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH). All the validation characteristics were meeting the acceptance criteria. Hence, the developed and validated method can be applied for the intended routine analysis.
... [4,5] Aspirin was estimated with mixtures in bulk and different pharmaceutical formulations by spectrophotometric methods [6][7][8][9][10] and by HPLC methods. [11][12][13][14][15][16][17][18][19][20][21][22][23][24][25][26][27][28] ASP was estimated from commercial samples by comparative study of spectroscopic and HPLC methods. [29] Besides, ASP was determined in the presence of dipyridamole using thin layer chromatography (TLC)-densitometric and HPLC methods. ...
Aspirin (ASP) and cilostazol (CST) are used as a combination in pharmaceutical formulations for treatment of strokes. Salicylic acid (SAL) is considered to be one of the main synthesis impurities and a degradation product of ASP. On the other hand, the main related impurities of CST are CST related A, B, and C (CST-RA, CST-RB, and CST-RC), respectively. Furthermore, as high efficiency and less elution are the basic requirements of high-speed chromatographic separation, so, a comparative study of two simple, precise, and accurate reversed-phase HPLC and UPLC methods was developed and validated for simultaneous estimation of ASP and CST in bulk and capsules in the presence of SAL, CST-RA, CST-RB, and CST-RC. A Eurospher II C18 (250 × 4.6 mm2, 5 µm) for HPLC method and an Agilent Zorbax Eclipse Plus C18 (50 × 2.1 mm2, 1.8 µm) for UPLC method were used. A gradient mobile phase of 20 mM anhydrous KH2PO4 buffer solution (containing 0.2% triethylamine (TEA), v/v) with pH adjusted to 2.9 using orthophosphoric acid (solution A) and acetonitrile (solution B) mixed in different proportions for HPLC and UPLC methods was prepared. Flow rate was set to 1.0 and 0.3 mL min−1 for HPLC and UPLC methods, respectively, and the detection was performed for both methods at 210 nm. It worth noting that the proposed UPLC-DAD assay exhibited relatively much more precision, sensitivity, specificity, and economic and chromatographic separation superiority than proposed HPLC-UV assay. Both developed methods were compared with reference methods to prove its applicability and are suitable for purity assessment of ASP and CST in bulk and capsules.
... Reviewing the literature in hand reveals that several techniques have been proposed for the simultaneous determination of ASP and DIP in their binary mixtures including spectrophotometry (12), spectrofluorimetry (13), TLC (14) and liquid chromatography (15,16). Other methods were reported for their determination in the presence of SAL by spectrophotometry (17), HPLC (18) and spectrofluorimetry along with HPLC (19). ...
Aspirin (ASP) and dipyridamole (DIP) are widely used as a combination in pharmaceutical formulations for treatment of strokes. Many of these formulations are containing tartaric acid as an excipient (in DIP pellets formulation for sustained release), which increases the probability of formation of dipyridamole tartaric acid ester impurity (DIP-I). On the other hand, salicylic acid (SAL) is considered to be one of the synthesis impurities and a degradation product of ASP. In this work, two chromatographic methods, namely, TLC-densitometry and HPLC, have been established and validated for simultaneous determination of ASP, DIP, SAL and DIP-I. Good separation was achieved by using silica gel as stationary phase and toluene–methanol–ethyl acetate (2:3:5, by volume) as mobile phase in the case of TLC-densitometry and Zorbax ODS column with mobile phase consisting of phosphate buffer (pH 3.3)–acetonitrile–triethylamine (40:60:0.03, by volume) for HPLC. Influence of different organic solvents in mobile phase composition has been studied to optimize the separation efficiency in TLC densitometry. Moreover, factors affecting the efficiency of HPLC, like pH of the buffer used, organic solvent ratio in the mobile phase and flow rate, have been carefully studied using one variable at a time approach. Finally, the proposed methods were validated as per ICH guidelines.
... Literature survey also reveals that no UV method is reported for simultaneous estimation of TIC and ASP in combination therefore, in the present work, a successful attempt has been made to estimate both these drugs simultaneously by Simultaneous Equation Method and absorption ratio Method, therefore the aim of the study was to develop simple, rapid, accurate, reproducible and economic Simultaneous estimation of TIC and ASP from its formulation. [6][7][8][9][10][11][12][13] The proposed methods were validated as per the International Conference on Harmonization (ICH) analytical method validation guidelines. [14][15] MATERIALS AND METHODS Pure sample of Aspirin and Ticlopidine Hydrochloride was kindly supplied by the Aarti Drugs Ltd. ...
A simple, accurate, precise, reproducible and economical analytical method was develop and validated. Spectrophotometric estimation of Ticlopidine Hydrochloride and Aspirin in tablet formulation 0.1N HCl was used as solvent. Two simple spectrophotometric methods have been developed. Method-I absorption ratio at 221.4 nm and 228 nm. Method-II simultaneous equation method which was carried out at the wavelength of 214 nm and 228 nm for Ticlopidine Hydrochloride and Aspirin respectively. The linearity range was found to be 5-25μg/ml and 2-10 μg/ml. The recovery studies were performed and the percentage recoveries were found to be 100.1% and 100.4% for Ticlopidine Hydrochloride and Aspirin respectively so, proposed methods were found to be simple, accurate, specific, linear, and reproducible.
... Although HPLC is a commonly used method in bioanalytical laboratories (Ahmad et al., 2011;Khan et al., 2011;Nama et al., 2011;Prakash et al., 2011), it is difficult to develop an HPLC method for ENT and LSP pharmacokinetic application, due to their low plasma concentration and endogenous interference. ...
A simple and highly selective method for determination of enalaprilat (ENT), lisinopril (LSP) and benazepril hydrochloride (BZP) in pharmaceutical dosage forms as well as spiked human plasma by ion chromatography with UV detection has been developed. ENT and LSP are compounds with little inherent hydrophobicity that make their analysis using HPLC essentially sophisticated necessitating either complex extraction procedures or especial detection methods. The method proposed is based upon ionization of those two drugs in basic medium to be well retained and readily resolved as dicarboxylic acid anions using IonPac AS11 (13 μm particle size, 4 × 250 mm, Dionex) anion exchange column adopting a very simple clean-up procedure via a single-step protein precipitation with UV detection at 215 nm. The three drugs were successfully determined in pharmaceutical dosage forms as well as in spiked human plasma with tyrosine as internal standard with a recovery approaching 100%. Adopting this proposed procedure, the analytes produce well shaped peaks with good linear relationship over the investigated concentration ranges and values of (r) higher than 0.998 for all drugs. ion level of200 ng ml-1 of the three drugs, therefore being satisfactory for their purposed analysis. The method was validated with respect to specificity, recovery, accuracy, precision and linearity. Moreover, the method could be applied to the determination of the drugs in pharmaceutical preparations. The method was validated with respect to specificity, recovery, accuracy, precision and linearity and the method proved applicable for routine fast analysis of the studied drugs.
Key words: Benazepril, enalaprilat, lisinopril, ion chromatography, pharmaceutical, plasma.
Simple RS method is developed and validated as reversed-phase chromatographic method for the identification and quantification of the dipyridamole related substances-A, B, C, D, E and F. Chromatographic separation has been achieved by using Shodex C18, 150 mm, 4.6 mm diameter, 5 µ column, using mobile phase 0.1 % of formic acid and acetonitrile by eluting in gradient with 1.0 ml flow, detection was achieved at 254 nm by maintaining 25 °C temperature for column. The method is validated as per the ICH guidelines. Linearity was recorded at various concentrations ranges 0.0100-6.0051 ppm for related substances A, B, C & 0.0040-2.4024 ppm of related substances D, E, F. Recovery RSD value of each related substance was <5.0 % (n=9). RS method for related substances in dipyridamole is found specific, linear, accurate, precise, rugged and robust hence the validated method is suitable to identify the related substances in dipyridamole drug. INTRODUCTION: Dipyridamole is chemically a derivative of pyrimido-pyrimidine nuclei, which has been developed to treat blood clot aggregation through the anti-platelet property by inhibiting platelets and endothelial adenosine uptake and inhibits the stimulation of both platelet-activating and collagen factors by triggering an accretion of cyclic adenosine monophosphate (cAMP) 1. Thorough literature reveals that only a few related substance analytical methods for dipyridamole and its related substances were reported.
