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Designed for the simultaneous estimation of Piracetam (PIRA) and Vinpocetine (VINP) combination a validated Reversed Phase-High-Performance Liquid Chromatography (RP-HPLC) method was
developed. The separation and analysis were performed on a reversed phase C18 column (250 mm×4.6 mm) with particle size 5 μm as the
stationary phase. The mobile phas...
Contexts in source publication
Context 1
... VINP is less as compared to PIRA. So, the wavelength of detection λmax 225 nm was selected to have a better simultaneous quantification of PIRA and VINP. The optimized chromatographic conditions were capable of resolving peak within short run time. The retention time of piracetam and vinpocetine was found to be 3.52 min and 7.41 min respectively (Fig. 2). A specific, reproducible and precise RP-HPLC method was developed and optimized for simultaneous estimation of PIRA and VINP. ...
Context 2
... RP-HPLC chromatogram of tablet sample analysis as depicted in Fig. No. 2. No sign of interference was observed from the commonly used tablet excipients that were added to the formulations. The result for % drug content of tablet was found to be 100.92 ± 0.68 for PIRA and 103.63 ± 0.02 and ...
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The objective was to develop and validate an easy, economical, fast, reliable, reproducible, precise and accurate reversed-phase high-performance liquid chromatography (RP-HPLC) method for the estimation of tapentadol hydrochloride (TAP, a mu opioid-receptor agonist,
and noradrenaline reuptake inhibitor) in bulk and pharmaceutical dosage form. The...
Citations
... This filtrate was appropriately diluted with methanol to achieve the solution concentration of 20µg/ml. By measuring the solutions absorbance and using the calibration curve, the amount of Vinpocetine was determined (35,36). ...
A quick, accurate, and cost-effective UV spectroscopy method was developed to estimate the Vinpocetine concentration in bulk, tablet dosage formulations and niosomes formulations, using a solvent ratio of (6:4) methanol: water. According to ICH guidelines, the proposed technique was validated and developed. In spite of linearity, precision, accuracy, specificity, LOD, and LOQ, like parameters were validated by using UV/visible spectroscopy technique to analyze a spiked Vinpocetine solution. The wavelength at which the drug's maximum absorbance peak was obtained at 274 nm and the solvents used as methanol: water (6:4 w/v). The ethanol injection technique was used to prepare niosomes to analyze Vinpocetine in UV / visible spectrophotometric method.During the inter and intra-day studies, it was discovered that the developed UV technique was accurate, with % relative standard deviation ranging from 0.27 to 0.46 and 0.26 to 0.46, respectively. Vinpocetine overall recovery percentage was discovered to be between 98.42 to 99.82 %. LOQ and LOD were calculated to estimate the method's sensitivity, and they were observed to be 0.4565 µg/ml and 0.1506 µg/ml, respectively. The estimation of Vinpocetine content in bulk form, marketed formulations and niosomes was achieved using the developed methodology. : A quick, accurate, and economical UV spectrophotometric method has been developed. As a result, the suggested UV spectroscopic technique has been developed to estimate the vinpocetine concentration in bulk, tablet dosage formulations, and niosomes formulations.
... For the study of linearity 25,26 , a series of specified amount of impurities and BRV concentrations has been prepared, ranging from LOQ to 200% of specification limit. Initially several linearity stock solutions has been prepared and finally the solution with the concentration is about 100ppm each of BRV, BRV-SS and 15ppm each of BRV-RR, BRV-RS has been injected into the chromatographic system. ...
Reverse-phase high-performance liquid chromatography method has been developed for the determination of brivaracetam (BRV) with its stereoisomeric impurities (BRV-SS), (BRV-RR) and (BRV-RS). Brivaracetam with its impurities has been eluted with good resolution using the chiral column, chiralpakIG (250 × 4.6mm, 5µ) column at the detection wavelength of 210nm with the flow rate of 0.50ml/minute. The separation was achieved with the mobile phase consisted of methanol: acetonitrile and trifluoroacetic acid in the volume ratio of 90:10:0.1. The column temperature was maintained at 30°C and detection wavelength was maintained at 210 nm. Brivaracetum (BRV), and stereoisomeric impurities, BRV-SS, BRV-RR and BRV-RS, were eluted at 13.829, 11.810, 10.448 and 9.449 min, respectively. The method showed adequate specificity, sensitivity, linearity, accuracy, precision, and robustness inline to ICH tripartite guidelines. The limit of detections were 0.2 μg/mL for BRV-SS and BRV-RR, for BRV-RS it was found 0.1μg/mL.The limit of quantification limits were 0.5μg/mL for BRV-SS, BRV-RR and for BRV-RS as well.The developed method was found to be linear over the concentration range of 0.5-20µg/mL for BRV-RS, for BRV-RR and BRV-RS it was 0.5-3µg/mLfor stereoisomeric impurities with a correlation coefficient of 0.999. The developed method was found precise (%RSD = 0.5%, 0.6% and 0.5% for BRV-SS, BRV-RR and BRV-RS,) accurate (with 96%-107% recovery) and found robust. The validation parameters of the developed method were within the limits as per the regulation of ICH Q2(R1) guidelines. Therefore, in this present method a good separation was achieved specifically for the identification of brivaracetam and its processed related stereoisomeric impurities using high performance liquid chromatography and found suitable for the quantification of stereoisomeric impurities of brivaracetam in bulk scale as well.
... Many HPLC methods have been reported for PIR analysis in pharmaceuticals, either on its own or in addition to impurities or other drugs. [37][38][39][40][41][42][43] Ketoprofen (KET) is 2-(3-benzoylphenyl) propionic acid. KET belongs is a nonsteroidal anti-inammatory drug (NSAID). ...
One of the main aims of green analytical chemistry (GAC) is the reduction of solvents and chemicals consumed. Recycling the mobile phase in chromatographic techniques provides an efficient way to implement GAC principles. However, this is not an easy job, particularly in the case of the gradient mode. Analysis of multi-pharmaceuticals for the same manufacturer using one mobile phase system dramatically reduces consumed solvents, time, and cost for pharmaceuticals analysis in quality control laboratories. This work is an attempt to reduce time, cost and effort needed for quality control analysis of several dosage forms produced by the same manufacturer. Our novel and green RP-HPLC method is able to separate and quantify a tertiary mixture of piracetam, ketoprofen and omeprazole produced by the same manufacturers. The analyst can easily quantify the three drugs in the three dosage forms in one run using the gradient elution mode of methanol and water (from 50% methanol to 85% methanol in ten minutes) with a flow rate 1.5 mL min−1 on a non-polar C18 column. Suitable dilutions were done for the working solution of the mixed pharmaceutical formulations prior to chromatographic analysis. This procedure will dramatically reduce the consumed solvents and save time and money during pharmaceutical analysis. The calibration ranges are (5–25), (5–25) and (3–20) μg mL−1 for the three studied drugs. The International Council for Harmonization (ICH) procedures were followed in the validation process and the results were evaluated in comparison with official HPLC methods, where no noteworthy differences were found. The green profile of the method and pictograms of AGREE and Green Analytical Procedure Index (GAPI) approaches proved the eco-friendly character for the studied drugs. The simultaneous quantitative analysis for Stimulan® and Hyposec® capsules, and Ketolgin® tablets from the Amoun Pharmaceutical Company, Egypt, can be accomplished via the novel method. Also, Memoral® ampoules, Topfam® tablets, and Gastroloc® capsules from Sigma Pharmaceutical Industries, Egypt, could be analyzed simultaneously. Omez® capsules and Ketogesic® tablets from the Pharaonia Pharmaceuticals, Egypt, could be determined simultaneously too. Applying this RP-HPLC method, a significant reduction of the total cost is assured as the required amount of solvent is noticeably decreased when performing multi-analyses in comparison to single component analysis.
... reverse phase high performance liquid chromatography (RP-HPLC) with UV-Vis detection (7)(8)(9)(10)(11)(12)(13)(14), ultra high performance liquid chromatography (UHPLC) with photodiode-array (PDA) detection (15,16), HPLC with chemical sensor (17), and HPLC with mass spectrometer detection (18,19). ...
Background:
Vinpocetine has been prescribed for the treatment of ischemic brain diseases for many years. The drug, which has side effects such as headache, flushing, and decreased blood pressure, is not found in nature, but it can be synthesized by several approaches.
Objective:
A simple, rapid, selective, stability-indicating high-performance liquid chromatographic (HPLC) method was developed for the simultaneous estimation of vinpocetine and their potential impurities in a tablet formulation.
Method:
Optimum HPLC conditions were tried to be determined by a statistical experimental design method. The proposed method was validated as per the ICH guidelines. Stress study was used to demonstrate the stability-indicating ability of the developed method in the quantification of vinpocetine and potential impurities within the same run.
Results:
According to multiresponse optimization using the Derringer's desirability function, the mobile phase consisted of an acetonitrile-phosphate buffer (pH 6.0) in the ratio of 65:35 (v/v) at a flow rate of 1.7 mL/min. Significant degradations were observed for the drug product under acid hydrolysis and alkali hydrolysis. The new method showed reasonable detection and quantification limits with good selectivity, precision, linearity, and recovery.
Conclusions:
These validation results have shown that this method is suitable for quantitative determination of vinpocetine and its impurities in quality control laboratories.
Highlights:
A reliable and rapid HPLC method optimized with response surface methodology and multiresponse optimization based on Derringer's desirability function was developed for the simultaneous analysis of vinpocetine and its impurities in a tablet formulation.
... Vinpocetine is a synthetic vinca's alkaloid derivate from Vinca rosea which has been widely used to treat cognitive diseases such as dementia in Alzheimer's disease. However, vinpocetine causes undesirable side-effects, such as stomach pain, nausea, sleep disturbances, headache, dizziness, nervousness and flushing [16][17][18][19][20] . Therefore, an alternative PDE1 inhibitor, especially from natural resources is needed. ...
... Vinpocetine administration for treatment of cognitive impairments, particularly for dementia in Alzheimer's disease has been clinically shown to be effective, despite of its side-effects 16,20 . Vinpocetine is known to improve and to enhance cognitive functions through the selective inhibition on PDE1 17,20 . ...
... Vinpocetine administration for treatment of cognitive impairments, particularly for dementia in Alzheimer's disease has been clinically shown to be effective, despite of its side-effects 16,20 . Vinpocetine is known to improve and to enhance cognitive functions through the selective inhibition on PDE1 17,20 . This enzyme inhibition increases cAMP/cGMP intracellular concentration where in contrast, patients with memory declines have a low neuronal cAMP/cGMP concentration compared to normal people 35,36 . ...
Vinpocetine (VIN) is a herbal supplement extracted from the periwinkle plant. It is a multi-action agent, which is used to treat various neurological disorders such as Alzheimer's and Parkinson's disease. Vinpocetine has also anti-inflammatory, analgesic, antioxidant property and treats various thinking and memory problems. Currently, vinpocetine is also available in the market as a dietary supplement to enhance cognition and memory. This profile explains the physicochemical properties, methods of preparation, content of related impurities and different spectroscopical behavior of vinpocetine. It also discusses the reported methods of analysis of the drug, which include Compendial Methods, Electrochemical Methods, Spectrophotometric Methods and Chromatographic Methods of analysis. Furthermore, this profile explains the stability of the drug subjected to stress conditions of acid, alkaline and photolytic degradation. In addition, the clinical applications of the drug, its uses, side effects, dosing information, pharmacokinetics and mechanism of action are also discussed.
Background
RP-LC is considered the most extensively used chromatographic technique in drug separation and quantification; yet its routine use shows increasing environmental challenges about energy consumption, solvent used and waste engendered. From this perception, efforts for Greening the developed RP-LC methods are focused on using of green solvents; reducing the amount of solvent used and waste produced.
Objective
The target of this work is to develop eco-friendly RP-LC method for the synchronous separation of six widely used drugs in the treatment of cerebrovascular and vestibular disorders namely; neurotropic Piracetam, antihistamines, Dimenhydrinate, Cinnarizine and Fluranizine, vasodilators Vincamine and Vinpocetine.
Method
Separation and quantification are accomplished at ambient temperature by isocratic elution mode using acetonitrile–0.2% triethylamine (85:15; by volume) as a mobile phase at a flow rate of 1.5 mL/min on Hypersil C18 column. UV detection and quantification are carried out at 225 nm.
Results
The method is fully validated per ICH guidelines, where all analytical parameters are within acceptable range, r > 0.9999, accuracy ≥99.55% and precision (0.02–0.97%).
Conclusion
The method is applied for the routine analysis of the cited drugs in their single and combined drug products and it is considered excellent in terms of greenness with respect to Eco-Scale assessment.
Highlights
As the routine use of RP-LC technique shows increasing environmental challenges, efforts for Greening are attempted focusing on the use of green solvents; reduce the amount of solvent used and waste produced. A simple eco-friendly RP-LC method for the synchronous separation of six widely used drugs in the treatment of cerebrovascular and vestibular disorders is developed. The method is fully validated per ICH guidelines, where all analytical parameter are within acceptable range. -The method is applied for the routine analysis of the cited drugs in their single and combined drug products.
Methyl 4-(4-aminostyryl) benzoate was successfully prepared and characterized. The compound was characterized via Fourier transform infrared (FT-IR), ¹H and ¹³C nuclear magnetic resonance (NMR) and UV-Visible analysis (UV-Vis). From the FT-IR result, it can be concluded that there is absorption of interest in carbon-carbon bond formation at 1624 cm⁻¹ and it is assigned as C=C. While ¹H NMR result showed the presence of methoxy resonance as singlet and the resonance of carbon-carbon bond formation at the expected regions. ¹³C showed the most deshielded regions appeared at carbons of carbonyl which is at δC 166.01 ppm and the carbons for methyl group at 50.97 ppm. In UV-Vis analysis, there are two important peaks that can be observed which is attributed in the presence of n-π* and π-π* electronic transition of C=O chromophores. The result suggested that the synthesized compound has great potential to act as precursor for formation of Schiff base derivatives. However, this study is still under preliminary stages on synthesizing Schiff base derivatives.
