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Determination and validation of UV-spectrophotometric method for estimation of paracetamol and diclofenac sodium in tablet dosage forms using hydrotropic solubilizing agents
Abstract
A novel, safe and sensitive method of spectrophotometric estimation in UV-region has been developed using 5 M urea solution as hydrotropic solubilizing agent for the quantitative determination of DCS and PC (Poorly water soluble drugs in tablet dosage form). DCS have λmax at 261.1 nm and obeys Beer's law in concentration range of 5-35 μg/ml. PC have λ max at 247.8 nm and obeys beer's law in concentration range of 5-35 μg/ml. Urea solution does not shows any absorption above 236 nm and does not show any interference in spectrophotometric estimations. All the results, parameters of the analysis were validated statistically.
... In the present investigation Lamivudine tablets have been estimated by BP method (spectrophotometric) which involved use of an organic solvent, methanol and also by the hydrotropic solubilization technique which involved use of Sodium benzoate as hydrotropic solubilizing agent. Author of the article and his research team has developed a UV Method development different pharmaceutical dosage form by hydrotropic agents [12][13][14][15][16][17][18][19][20][21][22][23]. The proposed method is new, accurate, simple and economic. ...
... A similar procedure was repeated using 1.0 M other hydrotropic solutions, in place of 5.0 M sodium benzoate solution, in all the cases. The results of analysis of recovery studies are presented in Table 2. 21,43,77,104,132,155,195 and 243 fold in case of lamivudine study proves that increase in solubilities of these three drugs in hydrotropic solutions are not due to alteration in pH, but are due to hydrotropic phenomenon. This indicates that the enhancement in the aqueous solubility of lamivudine in 5.0 M hydrotropic solutions was largely due to hydrotropy.Part A solution of drug was kept at room temperature for 48 h. ...
Ultraviolet absorption spectrophotometric method for the estimation of poorly water soluble drug like Lamivudine in pharmaceutical formulations has been developed. Aqueous solubility of this selected model drug was to a great extent (21 to 243fold) in 5.0 M sodium benzoate. Lamivudine shows maximum absorbance at 315 nm. Beer's law was obeyed in the concentration. Results of analysis were validated statistically and by recovery studies.
... The review of literature revealed that various analytical methods involving spectrophotometry [6][7][8][9][10][11] , HPLC [12][13][14][15][16][17][18][19] , HPTLC 20 have been reported for TOL in single form and in combination with other drugs. Several analytical methods have been reported for DFS in single form and in combination with other drugs including spectrophotometry [21][22][23][24][25] , HPLC [26][27][28][29][30][31][32] , LC-MS 33 , HPTLC 34 . ...
Two simple, accurate, precise, and specific spectrophotometric methods have been developed for the simultaneous determination of Tolperisone Hydrochloride (TOL) and Diclofenac Sodium (DFS) in its combined tablet dosage form by using methanol as a solvent. The first method is a dual-wavelength method which involves the estimation of TOL by absorbance difference at 267.19nm and 297.05nm, and DFS by absorbance difference at 241.26 nm and 266.4 nm. range of 10-50μg/ml for TOL and
DFS both. The mean % recoveries were found to be in the range of 99.63 – 100.67 % and 98.9 – 100.7 % for TOL and DFS respectively for the dual-wavelength method and in the range of 98.86 – 100.16% and 99.63 – 100.67% TOL and DFS respectively
for first order derivative method. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of TOL and DFS in their combined Tablet dosage form.
... On the other hand, the conventional classic, Paracetamol, is a widely used OTC (Over-the-counter) analgesicantipyretic molecule. Hence, in combination with Tapentadol, Paracetamol could be explored also in the management of chronic pain [15][16][17][18] . Therefore, this dynamic combination of Tapentadol and Paracetamol is a better alternative in comparison to other drug combinations of similar class such as Tramadol and Paracetamol because efficacy and safety goes hand-in-hand, and fewer side effect profile is a bonus point [19][20][21][22][23][24][25] . ...
The application of the ratio spectra derivative spectrophotometry to the simultaneous determination of Paracetamol (PCM) and Tapentadol (TAP) in combined pharmaceutical tablets is presented. The spectrophotometric procedure is based on the use of the first derivative of the ratio spectra obtained by dividing the absorption spectrum of the binary mixtures by a standard spectrum of one of the compounds. The first derivative amplitudes were measured at 220 and 232 nm for the assay of TAP and PCM, respectively. Calibration graphs were established for 1-5 μg mL-1 for TAP and 6.5-32.5 μg mL-1 for PCM in binary mixture. The detection limits for TAP and PCM were found 0.098 and 0.595 μg mL-1, respectively, while the quantification limits were 0.298 μg mL-1 for TAP and 1.805 μg/ml for PCM. The relative standard deviations were found to be less than 2%, indicating reasonable repeatability of both methods. The proposed methods were hence validated as per ICH guidelines and successfully applied to the determination of these drugs in commercial tablets.
... The literature survey revealed that various analytical methods involving UV spectrophotometry, HPTLC, HPLC have been reported for estimation of DIC alone or in combination with other drugs. [6][7][8] Hence an attempt has been made to develop simple, sensitive, rapid, precise, economical and accurate UV method to analyze the drugs smoothly. ...
Abstract: A simple, efficient, precise and accurate spectroscopic method has been developed and validated for quantitative
estimation of diclofenac sodiumin bulk and pharmaceutical dosage form. Diclofenac standard solution was scanned in the UV
rang (400-200 nm) in a 1 cm quartz cell in a double beam UV spectrophotometer. The absorption maxima of diclofenac were
found to be 276.20 nm. The method obeys beers law in the concentration range from 10- 30 μg/ml. The correlation coefficient
was found to be 0.9995 and regression of the curve was found y = 0.0324x + 0.0021 with excellent recovery 98.72-99.86%. Limit
of detection and limit of quantitation were found to be 1.03 mg/ml and 3.12 mg/ml respectively. The method was validated for
several parameters like accuracy, precision as per ICH guidelines. Value of % RSD and % recovery was found satisfactory, hence
the proposed method is precise, accurate and economical hence can be used for routine analysis of diclofenac sodium.
... Salleh, M. Nazrul Hakim when tested with the present of piroxicam as interference in diclofenac drug sample at 1:1 ration, indicating present method is free from the effect of interference. When compared to other spectroscopic methods [7, 9, 10], present method demonstrated less analysis time due to the simple experimental procedure. There was also a lower waste generation as no addition of chemical reagent is required throughout the procedure. ...
... [19] In the literature, several methods were reported for estimation of poorly water-soluble drugs using hydrotropic solubilizing agents. [20][21][22] Therefore, it was thought useful to utilize this hydrotropic solution to extract out the drug from fine powder of tablets to carry out spectrophotometric estimation. ...
This study was designed to develop and validate two simple, rapid, and economical UV-spectrophotometric and the first-order derivative methods using the area under curve method for estimation of diacerein in bulk and in capsule formulation.
In this study, hydrotrophic solution of 8 M urea and 0.5 M potassium citrate were employed as the solubilizing agent to solubilize a poorly water-soluble drug, diacerein. In the UV-spectrophotometry method, two wavelengths 252.0 nm and 266.2 nm and in the first-order derivative spectrophotometric methods two wavelengths 259.4 nm and 274.2 nm in 8 M urea and two wavelengths 247.8 nm and 267.4 nm in the UV-spectrophotometry method and in the first-order derivative spectrophotometric methods two wavelengths 259.2 nm and 274.2 nm in 0.5 M potassium citrate were selected for determination of areas.
Hydrotrophic agents used did not interfere in spectrophotometric analysis of diacerein. Diacerein followed linearity in the concentration range of 2-12 μg/mL with a coefficient correlation of 0.999 for both methods.
The amount of drugs estimated by both proposed methods are in good accord with label claim. The % RSD value in recovery, precision, and ruggedness studies are found to be less than 2 indicate that the method is accurate, precise, and rugged.
... Out of various methods available to increase water solubility of lipophillic drugs hydrotropy is an advanced and most successful method [2], in which solubility of poorly water soluble drug is increased by utilizing the highly water soluble substances. The agents used to increase the solubility of poorly water soluble drug in aqueous medium are known as hydrotropic agent, like sodium benzoate, niacinamide, sodium citrate, sodium acetate and - [3][4][5][6][7]. It is also known that the side effects of some drugs are the result of their poor solubility. ...
The solubility aspect of poorly water-soluble drugs is one of the biggest problems in their spectrophotometric analysis
and thus required to increase it through application of various solubility enhancement method. Hydrotropy is one of the
detrimental methods in which various salts are used to increase the solubility of drug like salicylic acid in water. The
objective of the present study was to employ the hydrotropic solutions of sodium citrate to enhance the solubility of
salicylic acid in water and prepare aliquots for UV spectroscopic analysis. We have found that the solubility enhancement
is more than 85 folds. Results of the analysis were validated statistically. After performing the experiment, it was found
that the amount of Salicylic acid estimated in pure sample by Indian Pharmacopoeial method was 98.94 ± 1.803 and it
was found to be 99.77± 1.932, by the proposed method of analysis using 1.25 M sodium citrate solution. In the present
investigation, it was found that using hydrotropy the solubility and UV analysis of salicylic acid is increased in aqueous
solvents.
This review explores sustainable strategies for enhancing the solubility of poorly water-soluble pharmaceutical active ingredients (PAIs), focusing on hydrotropy and co-solvency, while comparing their effectiveness, sustainability, and applicability in analytical chemistry, particularly within the frameworks of green and white analytical chemistry (GAC and WAC). Methods like hydrotropy, co-solvency, solid dispersions, and pH modification are discussed, each with distinct advantages and limitations. Hydrotropy, introduced by Carl A. Neuberg in 1916, enhances solubility without altering a drug's UV measurement range and is known for its eco-friendliness, stability, and scalability. Co-solvency modifies the solvent environment using solvents like ethanol but poses environmental concerns. Hydrotropy is safer and more scalable, though it requires more additives, while co-solvency is cost-effective but presents toxicity and precipitation risks. The environmental and safety benefits of hydrotropic solvents align with global sustainability initiatives like the UN SDGs. A case study comparing two UV methods (one with organic solvents and another with hydrotropic solvents) showed hydrotropy's superiority in sensitivity, stability, and sustainability, achieving a sustainability score of 71 % versus 29 % for methanol. The review also highlights the synergistic effects of multiple hydrotropic agents in improving solubility and drug stability. Overall, hydrotropy, particularly when combined with other solubility-enhancing techniques, represents a promising, sustainable approach for improving PAI solubility, offering significant safety, environmental, and economic benefits over traditional organic solvents.
The main objective of this study was to improve the aqueous solubility of Paracetamol and Domperidone using hydrotropic agents and to develop a validated method for their simultaneous estimation in pharmaceutical formulations using UV spectrophotometry. Paracetamol and Domperidone were sourced from Sigma Pharmaceuticals and Akums Pharma, respectively. Urea, sodium benzoate, niacinamide, sodium acetate, and sodium citrate were used as hydrotropic agents. The solubility of the drugs was determined using hydrotropic solutions and UV-visible spectrophotometry was employed to assess drug concentrations. Calibration curves for both drugs were prepared and regression equations were derived. The method was validated through statistical analysis of precision, recovery, and repeatability. The solubility of both Paracetamol and Domperidone improved significantly in the presence of hydrotropic agents, particularly urea (8 M). The solubility enhancement ratios were calculated, confirming the improved solubility. UV-visible spectrophotometric analysis showed linearity for Paracetamol (r² = 0.997) and Domperidone (r² = 0.995) in their respective concentration ranges. The regression equations were Y = 0.030 conc. + 0.014 for Paracetamol and Y = 0.098 conc. + 0.030 for Domperidone. The method was validated according to ICH guidelines. Recovery studies showed over 99% recovery for both drugs, indicating accuracy. Intra-day and inter-day precision, as well as analyst-to-analyst variability, were within acceptable limits (RSD < 1%). The solubility of Paracetamol and Domperidone was significantly enhanced using hydrotropic agents, with urea providing the best results. The developed UV spectrophotometric method allowed for the simultaneous estimation of both drugs, showing high precision and accuracy. The method was robust, with consistent results across different conditions and analysts. In conclusion, the study successfully enhanced the solubility of Paracetamol and Domperidone using hydrotropic agents. The developed UV spectrophotometric method for their simultaneous estimation was found to be simple, accurate and precise, making it suitable for routine analysis of pharmaceutical formulation. (2024) Solubility enhancement and estimation of paracetamol and domperidone by hydrotropic agents.
The aim of the study was to develop a simple, specific, precise, rapid, and accurate reversed-phase HPLC method and validate it for simultaneous estimation of Tolperisone hydrochloride (TOL) and Diclofenac sodium (DFS) in tablet dosage forms. The separation was achieved by Hyperchrom ODS-BP C18 column (200 mm x 4.6 mm, 5.0μm) using methanol: water (pH 2.7 adjusted with orthophosphoric acid)(90:10 v/v) as eluent, at a flow rate of 1 ml/min. Detection was carried out at wavelength 272 nm. The retention times of TOL and DFS were 1.96 min and 3.55 min respectively. The linearity was established over the concentration range of 9-72 μg/ml and 3-24 μg/ml with correlation coefficients (R2) 0.994 and 0.994 for TOL and DFS respectively. The mean recoveries were found to be in the range of 98.75-101.3% and 98.5-100.32% for TOL and DFS respectively. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of TOL and DFS their combined tablet dosage form.
Hydrotropic solubilization is a technique that can be used to improve the solubility of drugs that are poorly soluble. This technique involves adding a large amount of a second solute, known as a hydrotrope, which increases the aqueous solubility of the poorly soluble drug. Hydrotropes such as sodium citrate, sodium benzoate, and urea have been shown to be effective in enhancing the solubility of poorly soluble drugs. This technique has several advantages over other solubility enhancement techniques, including its cost-effectiveness, eco-friendliness, and the fact that it does not require chemical modification of hydrophobic drugs or the use of organic solvents. Hydrotropic agents are now being used to develop various dosage forms, including solid dispersions, mouth-dissolving tablets, and injections, to improve poorly water-soluble drugs' therapeutic effectiveness and bioavailability. This review paper will provide an overview of hydrotropic solubilization techniques.
In this ever-growing world, it is crucial to improve upon the formulations in terms of potency, patient acceptability, fewer side effects, and quicker relief. Due to these requirements, the market is flooded with various combination dosage forms, with a constant increase in number. Paracetamol is a commonly used non-steroidal anti-inflammatory drug (NSAID) that has antipyretic and analgesic action. This drug is available in a wide range of combinations. It acts by inhibiting the production of prostaglandins, which combat pain and inflammation. A simultaneous multicomponent analysis is used to determine the estimation of medicines that are available in combination. Different analytical techniques are available for their determination, one of which includes the use of UV spectrophotometric methods. This review focuses on a variety of paracetamol combinations with drugs like Domperidone, Aceclofenac, Diclofenac Sodium, Etodolac, Ibuprofen, Piroxicam, Caffeine, Aspirin, and their simultaneous estimation by different UV methods viz. Simultaneous equation method, Absorbance ratio (Q-Analysis), Difference spectrophotometry, Derivative spectroscopy method, and a few other chemometric methods. This manuscript would provide the platform to have exhaustive literature on methods used for the estimation of paracetamol with different drugs using a spectrophotometer. It would help the researchers and scholars who are working in the area.
Second order derivative spectroscopy method was developed and validated for the simultaneous estimation of Diclofenac sodium (DFS) and Serratiopeptidase (SPD) in bulk and tablet dosage form. Accurate and Précised UV Spectrophotometric method with good sensitivity has been developed for simultaneous estimation of DFS and SPD. The method employs Second order derivative based on the measurement of absorbance of DFS at ZCP 264.20 nm and SPD at ZCP 295.20 nm. The calibration curve was linear in a concentration range of 5-30 μg/ml for DFS and 25-150 μg/ml for SPD. The developed method was validated as per ICH guideline, for its accuracy, precision, LOD, LOQ and the results were found to be satisfactory, thus the method is specific, rapid and simple with good sensitivity for estimation of DFS and SPD in marketed dosage form.
This volume focuses on the most recent trends for greening analytical activities beginning with an introduction to green analytical chemistry followed by a discussion of green analytical chemistry metrics and life-cycle assessment approach to analytical method development. The chapters discuss two main topics; first is the most recent techniques for greening sample pretreatment steps, and second is modern trends for tailoring analytical techniques and instrumentation to implement the green analytical chemistry concept. The role of different kinds of green solvents, such as ionic liquids, supercritical fluids, deep eutectic solvents, bio-based solvents, and surfactants, as well as nanomaterials and green sorption materials in greening sample extraction steps is also a focus of this book. Furthermore, different approaches for greening chromatography as a key analytical technique are discussed. The applications of nanomaterials in analytical procedures are deeply reviewed, and miniaturization of spectrometers is also discussed as a recently evolved approach for efficient green on-site analysis. This book will appeal to a wide readership of academic and industrial researchers in different fields. It can be used in the classroom for undergraduate and postgraduate students focusing on the development of new analytical procedures for organic and inorganic compounds determination in different kinds of samples characterized by complex matrices composition. The book will also be useful for researchers that are interested in both chemical analysis and environment protection.
Ionic liquids are those ionic compounds which are liquid below 100 °C and are a combination of organic cations and inorganic/organic anions. They have wide potential to be used as solvents, extraction systems especially for biomedical applications. The past two decades have witnessed exponential rise in publications wherein ionic liquids have found applications in metal ion detection by coordination. This overview gives you a brief insight into the use of different ionic liquids for metal ion analysis.KeywordsIonic liquidOrganic ionsMetal chelationCoordinating ionsMetal extraction
There has been an exponential rise in chemical research since past three decades, which has witnessed an equal growth in the use of toxic and detrimental solvents, reagents, and reactants, leading to long-term environmental damage. Thereafter, with invent and advancement in green chemistry perspective, there has been a slight shift toward utilization of green chemistry principles in research, devolvement, and implementation. But the past decade has witnessed an immense rise in the use of green analytical chemistry owing to recent development in materials and methods that support the green concept.KeywordsGreen analytical chemistryGreen approachesTwelve Principles of Green analytical chemistryEco-friendly techniquesGreen chemistrySample preparationGAPINEMI
An acceptable, safe, and green technique for solubilization of poorly soluble drugs is the major important initial step for their handling through analytical work. Various procedures have been applied to enhance the aqueous solubility of such drugs. The major disadvantages of the use of organic solvents are that their volatility issues, as well as their considerable toxicity and cost. Hydrotropism technology and hydrotropic are considered as the green, convenient, and alternative procedures to achieve a step of solubility. In this chapter, we tried to introduce some topics related to the phenomenon of hydrotropy, its strategies, designs, and examples of these solvents that have been achieved to increase the solubility of some poorly water-soluble drugs. Urea and its derivatives, organic metal salts and acids, aromatic anionic and nonionic alcohols, alkaloids, aromatic cationic solutes, and anionic, cationic, nonionic, and amphoteric surfactants are categorical examples of the used hydrotropes’ solvents in various published analytical methods. Moreover, the updated direct, indirect, and derivatized spectrophotometric and titrimetric methods involving the solubility enhancement of various poorly water-soluble drugs using hydrotropic phenomena were sorted throughout this chapter.KeywordsGreen solubilizationHydrotropism technologyHydrotropic solventUrea and its derivativesDerivative spectrophotometric and titrimetric methods
Analytical chemistry plays a fundamental role in our society, being involved in drug manufacturing, medical diagnosis, industrial process control, environmental monitoring, food production, and soil analysis. However chemical analysis is usually associated with the usage of toxic substances or generation of waste, which can impact badly the environment. This has driven the need for green analytical chemistry, replacing the traditional chemical methods with other new technologies including in vivo analysis. Infrared spectroscopy is a one of the most clean and accurate methods that can be considered for green analytical chemistry. Infrared benchtop spectrometers have proven over that last decades to replace the chemical methods in many applications. However, their size and cost still cannot enable the ubiquitous chemical analysis using spectrometers. Recently, miniaturization of spectrometers has been evolved which led to many commercial products at a much less cost and with still a good performance. This opens the door for on-site spectral sensing solutions to enable ubiquitous green analytical chemistry.In this chapter, the basic concept of material spectroscopic analysis is introduced. For the application of this concept, different configurations for the spectral sensor solution as well as the sample handling are discussed. Based on this discussion, the building blocks as well as the performance of these sensors are explained indicating their main features and engineering characteristics. The simple analysis presented in this chapter allows quantitative evaluation of these sensors as ubiquitous solutions in the analytical chemistry different applications. The recent development of the miniaturized forms of these solutions present currently in the market/literature are then surveyed and critically compared at the end of this chapter.KeywordsSpectrometrySpectroscopyInfraredMiniature spectrometersAnalytical chemistry
Two non-steroidal anti-inflammatory drugs, ketoprofen and diclofenac sodium could be determined spectrofluorimetrically in their pure forms and different dosage forms using acriflavine reagent. It was found that the quenching of acriflavine fluorescence is going linearly with increasing the concentration over the ranges of 1.0-10.0 μg/mL for both ketoprofen and diclofenac sodium. The proposed method was studied to attain the optimum conditions with maximum sensitivity and precision without harming the environment. A proposal for the reaction mechanism was postulated depending on ion-association complex formation between acriflavine and each of the studied drugs in 1:1 ratio. International council of harmonization (ICH) guidelines were followed to validate the method. The lowest amount that could be detected by the proposed method is 0.28 and 0.48 μg/mL for both ketoprofen and diclofenac sodium, respectively. It was found that no significant difference between the proposed and comparison methods as indicated from the calculated statistical values.
PurposeParacetamol is a well-known OTC drug, and several combinations are available in the market. The numbers of chromatography methods were published for analysis of combined pharmaceutical dosage form of paracetamol. But every combination needs separate and dedicated chromatography condition for analysis. Hence, a chromatography method was developed for simultaneous estimation of some combined pharmaceutical dosage form of paracetamol using QRM and DoE-based quality by design approach.Methods
Quality risk management (QRM) was done by method risk parameter identification and assessment. The eleven potentially critical method risk parameters were screened for their main effect on the resolution of peaks by Placket Burman design. Further, three critical method risk parameters were analysed for their effect on the resolution of peaks by Box–Behnken design. Method operable design region (MODR) was navigated for optimisation of chromatography method. The chromatography method was used for simultaneous estimation of six combined dosage forms of paracetamol with different drugs.ResultsAfter QRM and DoE, mobile phase composition, the volume of acid, and plate activation temperature were found to be critical method parameters and optimised by the navigation of MODR. The optimised method gave results of the assay in agreement with the labelled claim of the dosage form.Conclusion
The developed method can fulfil a requirement of six different chromatography methods for the analysis of combined dosage forms of paracetamol. Hence, the developed chromatography method is versatile, economical, eco-friendly, and robust (VEER) for the simultaneous analysis of six combined dosage forms of paracetamol.
The hydrotropy though existing as precisely used scientific approach assisting solubilization for all. It took 66 long years to use the concept in drug analysis since its inception in 1916 and first use for facilitation of drug solubility toward better pharmaceutical analysis in 1982. Considering the unending importance in pharmaceutical sciences and thereby in analysis, it’s a necessity to comprehensively outlook the origin, evolution, cumulative trend and precise applications in pharmaceutical analysis. Achieved hereby with chronological and comparative assessment of the studies published pertaining to solubility enhancement of poorly soluble drugs with use of hydrotropic agents alone or in combination for assisting pharmaceutical analysis. The thorough literature searches resulted into 77 references over a span of about 38 years. This comprehensive review critically evaluates existing literature; to our surprise we found Ibuprofen sodium, Lignocaine, Niacinamide and Metformin HCl as atypical hydrotropic agents. We also compared herein mono and mixed approaches which indicated prevalence of mono - hydrotropy over mixed. The possible mechanisms behind solubilization are presented for an additional insight. An essential effort has been made to state arbitrary classification to assist in future applications. The obvious purpose of this study was to collectively evaluate the crucial role of hydrotropic agents in pharmaceutical analyses for better drug delivery. This comprehensive review covers all details since inception to the updates till date which will definitely act as appropriate guideline for pharmaceutical analyst’s in need of hydrotropy to assist pharmaceutical analysis for therapies today and tomorrow.
Derivative spectrophotometry, which is primarily based on the first and second derivative spectra of absorption, was applied for individual and simultaneous spectrophotometric determination of diclofenac sodium (DS) and nicotinamide (NAM) in the ultraviolet region. The method depends on 1st and 2nd derivative UV spectrophotometry, with the amplitude of peak-to-base line, peak to peak, the area under peak at selected spectrum intervals and zero-crossing at certain wavelengths for each compound measurement. Under optimal conditions, a linear working range of 5-80 μg.ml-1 and 10-140 μg.ml-1 for (DS) and (NAM) with correlation coefficient R2 between 0.9938-0.9998. The mean % recoveries were found to be in the range of 97.95-102.50 % for two drugs. The proposed technique has been effectively applied to the estimation of (DS) and (NAM) in pharmaceutical formulations.
Derivative spectrophotometry, which is primarily based on the first and second derivative spectra of absorption, was applied for individual and simultaneous spectrophotometric determination of Diclofenac sodium (DS) and nicotinamide (NAM) in the ultraviolet region. The method depends on 1st and 2nd derivative UV spectrophotometry, with the amplitude of peak-to-base line, peak to peak, the area under peak at selected spectrum intervals and zero-crossing at certain wavelengths for each compound measurement. Under optimal conditions, a linear working range of 5-80 μg.ml-1 and 10-140 μg.ml-1 for (DS) and (NAM) with correlation coefficient R2 between 0.9938-0.9998. The mean % recoveries were found to be in the range of 97.95-102.50 % for two drugs. The proposed technique has been effectively applied to the estimation of (DS) and (NAM) in pharmaceutical formulations.
A rapid, specific and economic UV spectrophotometric method has been developed using solvent composed of methanol: water (10:90) to determine the content of Methocarbamol and Diclofenac sodium in injection dosage form. Estimation of Methocarbamol and Diclofenac sodium was carried out at 274.11 nm (max. wavelength of MET) and 282.45 nm (isoabsorptive point) for Absorbance Ratio method and 223.92 nm for Diclofenac sodium (ZCP of Methocarbamol) and 281.69 nm for Methocarbamol (ZCP of Diclofenac sodium) for First order derivative spectroscopy method. Methocarbamol and Diclofenac sodium were found to be linear over the range of 12-60 µg/ml and 2-10 µg/ml respectively for both the methods. The method was validated statistically and studied for linearity, precision, accuracy, LOD and LOQ. The obtained results proved the method can be employed for the routine analysis of Methocarbamol and Diclofenac sodium in injection dosage form.
A simple, accurate, precise and specific spectrophotometric method have been developed for simultaneous determination of Tolperisone Hydrochloride (TOL) and Diclofenac Sodium (DFS) in its combined tablet dosage form by using methanol as a solvent. The method involves solving of simultaneous equation based on measurement of absorbance at two wavelengths at 254 nm and 282 nm. Method follows Beer's linearity in the range of 5-35μg/ml for TOL and DFS both. The mean % recoveries were found to be in the range of 99.35 - 100.4% and 98.70 - 100.20 % for TOL and DFS respectively. Limit of Detection and quantitation was found to be 0.101μg/ml and 0.306μg/ml for TOL and 0.120μg/ml and 0.364μg/ml for DFS respectively. Assay results of market formulation were found to be 99.70 and 99.40 % for TOL and DFS respectively. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of TOL and DFS in their combined Tablet dosage form.
Two simple, rapid, precise and accurate spectrophotometric methods have been developed for simultaneous analysis of Paracetamol (PCM) and Pamabrom in bulk drugs and pharmaceutical formulation. Method A, Second derivative zero crossing spectrophotometry which involve conversion of zero order spectra into second order derivative spectra and measure zero cross points, at 227 nm PCM has zero cross point so Pamabrom can be measured and at 268 nm Pamabrom has zero crossing point so PCM can be measured. The concentrations can be calculated from the derived equations. Method B, Single divisor ratio derivative spectrophotometry, in which zero order spectra of one drug was divided by minimum concentration of other drug which give higher R2 value and ratio spectra of drug was converted into first order spectra for better visualisation. Amplitude at 270.9 nm and 231.9 nm were selected in the ratio derivative spectra to determine Pamabrom and PCM, respectively Developed methods were validated according to ICH guidelinesQ2 (R1)[11]. The calibration graph follows Beer's law in the range of 1 to 35μg/ml for Pamabrom and 5.0 to 30 μg/ml for PCM with R2 value greater than 0.999. Accuracy of all methods wasdetermined by recovery studies and showed % recovery between 98 to 102%. Intraday and interday precision was checked for all methods and mean %RSD was found to be less than 2 for all the methods. The methods were successfully applied for estimation of Pamabrom and PCM in pharmaceutical formulation.
This study was aimed to develop a simple and reproducible spectrophotometric method for the characterization of diclofenac sodium (DS) and to evaluate the efficacy of orally administered liposome encapsulated as well as free form DS in animal model. A simple, rapid and economical spectrophotometric analytical procedure with estimation in UV-visible region was performed on DS using dimethyl sulfoxide as solvent. Parameters such as time, temperature and types of solvent were studied for 20 μg/mL DS solution at 295 nm. All parameters and results of analysis were statistically validated. Liposome-encapsulated and free form DS samples were subjected to characterization study that includes entrapment efficacy determination and particle size analysis. Drug samples were further tested for their in vivo anti-inflammatory efficacy using histamine-induced paw edema test. Under optimized parameters, the Beer's law is obeyed in range of 0.625-40 μg/mL at λnax 295 nm. A linear working range of 5-35 μg/mL with regression coefficient of 0.9978 was obtained by using seven triplicate analyses of drug samples at seven different concentrations. The limit of detection and limit of quantitation was 1.19 and 3.62 μg/mL, respectively. Result of characterization study showed that the optimum formulation, which has high entrapment efficacy of 87%, homogenous in size (polydispersity index 0.27), stable and reproducible, were obtained by using the Pro-Lipo Duo with 10 h hydration time and 16 mg/g DS. The liposome encapsulated DS resulted in significant (P < 0.05) inhibition up to 86% in histamine-induced paw edema test. Present study successfully demonstrated an optimized procedure as per ICH guidelines in detection and evaluation of DS. In addition, nano-encapsulation of DS using liposome was found to demonstrate a potential enhancement in therapeutic efficacy.
In the present investigation, cephalexin has been selected as a poorly water-soluble model drug. There was more than 6-fold enhancement in aqueous solubility of cephalexin by 8.0 M urea solution (as compared to aqueous solubility). This hydrotropic agent was employed to solubilize the drug from the fine powder of tablet formulations. The selected λ max for spectrophotometric estimation was 262 nm. The hydrotropic agent and the additives used in the manufacture of tablets did not interfere in the analysis. Proposed method is new, rapid, simple, accurate and reproducible. Statistical data prove the accuracy, reproducibility and the precision of the proposed method.
In the present investigation, hydrotropic solution of urea (10.0 M) was employed to solubilize amoxycillin trihydrate (a poorly water-soluble drug), from fine powder of its tablets, to carry out spectrophotometric analysis. Beer's law was obeyed in the concentration range of 50-350 μg/mL at 274 nm. Recovery studies and statistical data proved the accuracy, reproducibility and the precision of the proposed method. Presence of urea and commonly used tablet excipients did not interfere in the spectrophotometric estimation.
In the present investigation, tinidazole has been selected as a poorly water-soluble model drug. There was more than 60, 70 and 105 fold enhancement in aqueous solubility of tinidazole by 1.25 M sodium citrate, 4 M sodium acetate and 8 M urea solutions (as compared to aqueous solubility), respectively. These hydrotropic agents were employed to solubilize the drug from the fine powder of tablet formulations. The selected λmax for spectrophotometric estimation was 318 nm. The hydrotropic agents and the additives used in the manufacture of tablets did not interfere in the analysis. Proposed method is new, rapid, simple, accurate and reproducible. Statistical data proved the accuracy, reproducibility and the precision of the proposed method.
Quantitative estimation of poorly water-soluble drugs involves use of organic solvents. Major drawbacks of organic solvents include high cost, volatility and toxicity. In the present investigation, hydrotropic solubilization is employed to enhance the aqueous solubilities of poorly water-soluble drugs norfloxacin and tinidazole in two component tablet formulation for simultaneous spectrophotometric determination. Three simple, accurate and economical procedures employed are program in the multi-component mode of analysis of the instrument used, graphical absorbance ratio method and simultaneous equation method. All methods utilize 8.0 M urea solution as hydrotropic solubilizing agent. In the urea solution, norfloxacin and tinidazole show maximum absorbance at a wavelength of about 274 and 320.5 nm respectively and isobestic point is observed at 297.5 nm. The hydrotropic agent and additives used in the manufacture of tablets did not interfere in the analysis. The results of analysis have been validated statistically and by recovery studies.
Concentrated aqueous solutions of various hydrotropic agents like sodium salicylate, sodium benzoate, sodium citrate, sodium acetate, urea and nicotinamide have been observed to enhance aqueous solubilities of a large number of poorly water-soluble drugs. In the present investigation, paracetamol has been selected as a poorly water-soluble drug. There was more than 7-fold enhancement in aqueous solubility of paracetramol by 10.0 M urea solution (as compared to its aqueous solubility). This hydrotropic agent was employed to solubilize the drug from the fine powder of tablet formulations. The selected λmax for spectrophotometric estimation was 245 nm. The hydrotropic agent and additives used in the manufacture of tablets did not interfere in the analysis. Proposed method is new, rapid, simple, accurate and reproducible. Statistical data proved the accuracy, reproducibility and the precision of the proposed method.
In the present investigation, hydrotropic solubilization technique has been employed to solubilize the poorly water soluble antiinflammatory drug, ketoprofen (by 2.0 M sodium benzoate, 2.0 M sodium salicylate and 2.0 M sodium acetate solutions) and the poorly water soluble keratolytic drug, salicylic acid (by 2.0 M sodium benzoate, 8.0 M urea and 1.25 M sodium citrate solutions) for their titrimetric analyses The proposed method is new, simple, accurate and reproducible. Statistical data prove the accuracy, reproducibility and precision of the proposed method.