Precise Spectroscopic Method Research Articles

Simultaneous Estimation of Amlodipine and Atorvastatin Using UV-Spectroscopy Method

The simple, precise and accurate UV spectroscopic method has been developed for simultaneous estimation of amlodipine besylate and atorvastatin calcium. The developed simultaneous equation method is reproducible and economical. The wavelengths selected for measuring the absorbance of both drugs were 365 and 246 nm, respectively. In a concentration range of 2 to 10 μg/mL, amlodipine besylate and atorvastatin calcium exhibited linearity at their respective λmax of 365 and 246 nm as well as at the isoabsorptive point at 238 nm. Recovery studies showed recovery of >99.78% for amlodipine besylate and >99.36% for atorvastatin calcium, indicating method accuracy. The developed method is suggested for routine analysis because it is quick, easy, accurate, as well as sensitive and specific. The validation studies were carried out in accordance with the International Council of Harmonization (ICH) recommendations.

RGB-algorithm whiteness appraisal approach for quantitative determination of clopidogrel and aspirin in presence of salicylic acid as a degradation product based on proton NMR technique

A rapid, precise, and selective spectroscopic method based on the quantitative proton nuclear magnetic resonance (1H-qNMR) was developed to estimate aspirin and clopidogrel in their pharmaceutical dosages for the first time. The evolved method was utilized to estimate both drugs in presence of the aspirin degradation product, salicylic acid. Moreover, aspirin and clopidogrel were subjected to various stress conditions such as acid hydrolysis, alkali hydrolysis, water hydrolysis, H2O2 oxidation, and photodecomposition for studying the stability of both compounds under these stress conditions. The 1H-qNMR analyses of the analytes of interest were conducted using the internal standard phloroglucinol and the solvent dimethyl sulfoxide-d6. The NMR spectra showed a quantitative doublet of doublets (dd) signal of aspirin at 7.945 ppm, a doublet signal of clopidogrel at 6.875 ppm, and a dd signal of salicylic acid at 7.810 ppm. The internal standard phloroglucinol exhibited a singlet signal at 5.690 ppm. The results demonstrated the linearity (r2 > 0.999), accuracy, precision (RSD < 2.0 %), stability, selectivity, and specificity of the evolved method. Linearity was confirmed in the ranges of 0.05–3.0 mg/mL for aspirin, 0.15–10.0 mg/mL for clopidogrel, and 0.1–5.0 mg/mL for salicylic acid. The evolved method was efficiently applied to analyse aspirin and clopidogrel in their dosages with high %recovery. Moreover, The RGB algorithm technique was used to evaluate the whiteness profile of the suggested method; the findings confirmed the sustainability of the evolved method, which employed an ecological solvent, followed a simple and straightforward procedure, and avoided any pretreatment or labelling stages for the samples. All the aforementioned advantages gave the technique the privilege.

DEVELOPMENT OF AN ACCURATE UV SPECTROSCOPIC METHOD FOR TINIDAZOLE IN VAGINAL BUFFERS

A precise UV spectroscopic method was developed for accurately quantifying tinidazole (TNZ) using the Shimadzu 1900i UV spectrophotometer. Different sample solutions containing TNZ were scanned across a range of concentration 6 µg mL-1 to 26 µg mL-1 between 200-400 nm, generating overlay TNZ spectra showing an absorption maximum at 318nm in vaginal buffer which is made up of phosphate buffer (PB) 4.2 pH with 2% Tween 80® LR and 4 mL of methanol. The construction of a six-point calibration curve demonstrated the linearity of TNZ within the 6-26 µg mL-1 concentration range. The regression equation derived from this calibration curve was subsequently employed to accurately determine the concentration in accuracy studies. In the analysis of bulk TNZ, a recovery rate ranging from 98.41% to 102.28% was achieved. The analysis results were validated following ICH (International Council on Harmonization) guidelines and compiled with the required criteria and standards

Spectroscopic method to estimate 3-Acetyl-11-keto-β-boswellic acid in complex lipid nanocarriers and skin matrices

3-Acetyl-11-keto-β-boswellic acid (AKBA) is a phytoconstituent derived from Boswellia serrata extract. It shows anti-rheumatic activity by selectively and non-competitively inhibiting the 5-Lipoxygenase (5-LOX) enzyme. AKBA is utilized for complex nanocarriers for its effective topical delivery at the arthritic site. There is a demand to develop a rapid, sensitive, and economical UV–Visible spectroscopic method for AKBA, which can be utilized in nanoformulation designing and day-to-day analysis of in vitro and ex vivo samples. In this research work, an analytical method was developed for the estimation of AKBA in two solvent systems, methanol and phosphate buffer saline pH 7.4, using a UV–Visible spectrophotometer. Further, the developed method was validated for linearity, range, limit of detection, limit of quantification, accuracy, precision, solution stability, and specificity as per regulatory guidelines. The method exhibited a linearity range of 10–50 µg/mL in both media with the obtained value of the high correlation coefficient (>0.9995). Interday and intraday precision samples showed less than 2 % relative standard deviation (% RSD) that exhibited the reliability of the developed method. The accuracy study reflected the % recovery between 99 and 101 % in both media. Further, the developed method was explored to quantify AKBA in formulated lipid nanocarriers (LNCs) formulation. The methanol method was effectively used to estimate the entrapment efficiency in LNCs and skin retention of AKBA. For the quantification of AKBA in in vitro release and ex vivo permeation samples, the phosphate buffer saline pH 7.4 method was utilized. Results indicated that the method could quantify the AKBA in the presence of different sample matrices with reproducibility in nature. In conclusion, a sensitive, simple, economical, precise, and accurate UV–Visible spectroscopic method was developed and validated to quantify AKBA.

Derivative Spectroscopic Method and RP-HPLC Method Development and Validation of Levofloxacin hemihydrate

The present work describes the development of a simple, precise and accurate derivative spectroscopic and RP-HPLC method for the estimation of levofloxacin hemihydrate in the tablet dosage form. Levofloxacin hemihydrate showed absorption maxima at 287.36, 287.2 and 296.2nm in zero, first and second-order spectroscopic methods. The RP-HPLC method was optimized by using Orthophosphoric acid: acetonitrile: methanol (50: 20: 30) as solvent at 287nm. The methods showed linearity in the concentration range 1-5 and 2-10 µg/ ml and the correlation coefficient was 0.999 respectively. The method has been validated according to the ICH guidelines. The percentage relative standard deviation was found to be less than 2% in respect of both methods.

Development of simple, precise UV spectroscopic methods for the estimation of Lamotrigine in bulk and marketed tablet

Two Simple and precise UV spectroscopic methods were developed for the estimation of lamotrigine in bulk and marketed tablets. The methods developed by using two solvent systems viz., Acetonitrile: Distilled water (1:1) and Methanol: 0.1N HCl (3:1) were validated as per ICH guidelines. The two proposed solvent systems validated for linearity, accuracy, precision, robustness, ruggedness and solution stability. The percent recovery in the marketed tablet formulation was found to be good agreement with the label claim. The methods validated statistically and the results suggest these methods can employed for the routine analysis of lamotrigine in bulk and marketed tablet formulations.

Development of simple, precise UV spectroscopic methods for the estimation of Lamotrigine in bulk and marketed tablet

Development of simple, precise UV spectroscopic methods for the estimation of Lamotrigine in bulk and marketed tablet

DEVELOPMENT AND VALIDATION OF UV SPECTROSCOPIC METHOD FOR ESTIMATION OF ABACAVIR IN TABLET DOSAGE FORM

Objective: To develop and validate simple, rapid, linear, accurate, precise and economical UV Spectroscopic method for estimation of Abacavir in tablet dosage form.&#x0D; Methods: The drug is freely soluble in analytical grade methanol. The drug was identified in terms of solubility studies and on the basis of melting point done on the melting point apparatus of Equiptronics. It showed absorption maxima were determined in analytical grade methanol. The drug obeyed the Beer’s law and showed good correlation of concentration with absorption, which reflect in linearity. The UV spectroscopic method was developed for estimation of Abacavir in tablet dosage form and also validated as per ICH guidelines.&#x0D; Results: The drug is freely soluble in analytical grade methanol, slightly soluble in water and practically insoluble in ethanol. So, the analytical grade methanol is used as a diluent in method. The melting point of Abacavir was found to be 164-165 ˚C (uncorrected). It showed absorption maxima 256 nm in analytical grade methanol. On the basis of absorption spectrum the working concentration was set on 15µg/ml (PPM). The linearity was observed between 5-25 μg/ml (PPM). The results of analysis were validated by recovery studies. The recovery was found to be 98.75, 101 and 99.17% for three levels respectively. The % RSD for precision was found to be 0.32% and for Ruggedness is 0.46%&#x0D; Conclusion: A simple, rapid, linear, accurate, precise and economical UV Spectroscopic method has been developed for estimation of Abacavir in tablet dosage form. The method could be considered for the determination of Abacavir in quality control laboratories.

A rapid and precise spectroscopic method for detecting fipronil insecticide on solid surfaces

A rapid and precise spectroscopic method for detecting fipronil insecticide on solid surfaces

Development and validation of derivative UV spectroscopic method for simultaneous estimation of nicotinamide and tretinoin in their binary mixtures and pharmaceutical preparations

An accurate, precise, sensitive, and simple spectroscopic method was developed and validated for simultaneous quantification analysis of tretinoin (TRT) and nicotinamide (NCT) with a ratio of 1:40 (TRT: NCT) in a synthetic mixture from dermal pharmaceutical preparations (solution and cream). Wavelengths were chosen in the first and second-order derivatives which are valid for the determination of NCT with the existence of TRT and excipients of the tested pharmaceutical preparations. Wavelength 253 nm was picked for the first-order derivative. Wavelengths 245 and 269 nm were picked for the second derivative. All previous wavelengths were zero-crossing points for TRT and its pharmaceutical preparations. Zero-order spectroscopy was used to determine TRT at the wavelength 348 nm, where no interference with NCT or any substance in the previous pharmaceutical preparation. The linearity range was studied and found to be 20–120 μg/mL and 0.5–5.0 μg/mL for NCT and TRT respectively. The correlation coefficient was 0.9995–0.9999 for NCT and 0.9998–0.9999 for TRT. The limit of detection (LOD) and the limit of quantification (LOQ) of NCT were 1.510 μg/mL and 4.590 μg/mL respectively at the wavelength 269 nm of the second-order derivative.

UV Spectrophotometric Method Development and Validation of Lignocaine Hydrochloride in Bulk and Semisolid Dosage Form

Objective: A new, simple, sensitive, precise and reproducible UV spectroscopic method was developed for the estimation of Lignocaine Hydrochloride in bulk and Semisolid Formulation. Methods: The UV spectrum of Lignocaine Hydrochloride in RO water showed λ max at 228.8nm. Beer’s law is valid in the concentration range of 20-100µg/ml. This method was validated for linearity, accuracy, precision, ruggedness and robustness. Results: The method has demonstrated excellent linearity over the range of 20-100µg/ml with regression equation y = 0.0097x + 0.023 and regression correlation coefficient r2= 0.9992. Moreover, the method was found to be highly sensitive with LOD (3.55μg/ml) and LOQ (10.75μg/ml). Conclusion: Depending on results the given method can be successfully applied for assay of Lignocaine Hydrochloride in Semisolid formulation.

Determination of ketoprofen in tablet dosage forms by derivative IR spectroscopy

The study as a simple and rapid method has been described for determination of ketoprofen depending upon normal and first derivative IR Spectroscopy. The aim of this study is to develop a specific, precise and accurate spectroscopic methods that could be applied in quality control for the determination of ketoprofen in pharmaceutical formulations. Ketoprofen has been determined quantitatively in the range of (1000 to 4000)μg/ml depending on the measurement of transmittance for normal and its first derivative spectrum against the concentration with relative error+4.33% and 4.78% and RSD 1.15% and 1.37%, respectively. The values of r2of the both methods were 0.993 and 0.978, respectively. The methods have been applied for determination of ketoprofen in some pharmaceutical samples with recovery 97.691%.The obtained results were statistically compared to those of a reported HPLC technique and t-student's and F- tests at P=0.05 are calculated2SA1`

DEVELOPMENT AND VALIDATION OF UV SPECTROSCOPIC METHOD OF PALIPERIDONE PALMITATE IN BULK AND ITS APPLICATION FOR DRUG LOADING AND ENTRAPMENT EFFICIENCY ANALYSIS OF LONG-ACTING INJECTABLE MICROSPHERES

Objective: The objective of the current study was to develop simple, precise and cost-effective ultraviolet (UV) spectroscopic method for estimation of paliperidone palmitate (PP) as a bulk and in the polymeric depot dosage form.&#x0D; Methods: UV spectrophotometer with quartz sample cells and spectral manager software was used for analysis samples. 20 % Methanol in Mili-Q-Water was used as a solvent for the sample and standard preparations. Method validation was carried out as per ICH Q2 (R1) guidelines. Stress degradation studies were carried out to check the stability-indicating performance of the developed method. The validated method was applied for the estimation of the PP content of long-acting injectable microspheres of PP.&#x0D; Results: The wavelength of maximum absorption was found to be 283 nm. The proposed method was validated in the range of 5-30 µg/ml of PP. The mean recovery for 80%, 100% and 120% standard solution was found to be 99.03%, 99.21% and 99.35% respectively with less than 2% relative standard deviation (RSD). Intra-day and inter-day method precision ranged from 0.54 to 1.62% and 0.67 and 1.24% respectively. Limit of detection (LOD) and limit of quantitation (LOQ) were estimated to be 0.03 and 0.10 µg/ml respectively. The developed method was found to be robust and rugged. Stress degradation studies were carried out under acidic, alkaline, hydrolytic and oxidative and photo stress. The proposed method was capable to detect changes in assay due to stress conditions.&#x0D; Conclusion: The developed method was successfully employed for routine analysis of drug loading in long-acting injectable microspheres of PP.

Development and Validation of UV-Spectroscopic First Order Derivative Method for Simultaneous Estimation of Rosuvastatin Calcium and Teneligliptin Hydrobromide Hydrate in Synthetic Mixture

This work aimed to develop and validate a simple, accurate, precise, and reproducible spectroscopic method for simultaneous estimation of rosuvastatin calcium and teneligliptin hydrobromide hydrate by UV-Visible first-order derivative method. According to our present knowledge, no UV method was reported for combination of rosuvastatin and teneligliptin. So, in this work, it was decided to performed the first-order derivative method and it was validated as per ICH(Q2 R1) guideline. Rosuvastatin calcium and teneligliptin hydrobromide hydrate showed absorbance at the working wavelength of 230.03 nm (Zero crossing point of rosuvastatin calcium) and 222.66 nm (Zero crossing point of rosuvastatin calcium), respectively, using methanol as diluent. Linearity was found over the concentration range of 1-42 µg/ml for both drugs and correlation coefficients was 0.9995 and 0.9994, respectively. Accuracy was found between 98.91%-101.13% and 99.38%-100.25% for rosuvastatin calcium and teneligliptin hydrobromide hydrate, respectively. LOD was found to be 0.213µg/ml and 0.120 µg/ml for rosuvastatin calcium and teneligliptin hydrobromide hydrate respectively. LOQ was found to be 0.646 µg/ml and 0.3648 µg/ml for rosuvastatin calcium and teneligliptin hydrobromide hydrate, respectively. The result revealed that the developed method is suitable for analysis of determining rosuvastatin calcium and teneligliptin hydrobromide hydrate in a binery mixture.

Smart spectrophotometric methods for the simultaneous determination of newly co-formulated hypoglycemic drugs in binary mixtures

Achieving good glycemic control in patients with type II diabetes mellitus is essential for preventing both microvascular and macrovascular complications. Combination therapy represents the principle strategy for successful long term control of type II diabetes mellitus with minimal complications. Two sensitive, precise and non-destructive spectroscopic methods were developed for the simultaneous estimation of two new co-formulated hypoglycemic drugs; canagliflozin/metformin (CAG/MEF) and empagliflozin/linagliptin (EMG/LIG) in tablets with no need of previous separation. The first method was amplitude modulation (a normalized spectra-based UV spectrophotometric method) for the analysis of (CAG/MEF) binary mixture. The amplitude of the constant at the plateau region at (264–310 nm) on the ratio spectrum was measured and used for the determination of CAG concentration in the mixture. On the other hand, MEF was estimated by subtracting the previously obtained amplitude from the total amplitude of CAG and MEF at the isosbestic point (λiso) at 250 nm. The second method was chemometric-assisted FTIR spectrophotometric method for the determination of (EMG/LIG) binary mixture. (EMG/LIG) mixture in chloroform was analyzed using FTIR in the region 4000–400 cm−1. The spectral region 3900–2900 cm−1 was selected for (EMG/LIG) determination using principal component regression and partial least squares chemometric methods. The methods were validated according to ICH guidelines. The studied drugs were successfully determined in tablets applying the developed methods. Validation parameters were in agreement with acceptance limits, ensuring methods accuracy and selectivity. Besides, no significant difference was obtained by statistically comparing the obtained results with the reported one.

A Validated high Performance Liquid Chromatographic Method for the Quantification of Favipiravir by PDA Detector

Favipiravir is an antiviral agent showing activity for the treatment of various life threatening viruses such as Ebola virus, Lassa virus and also recent virus for COVID-19. It is a pyrazine carboxamide derivative with activity against RNA viruses which targets RNA-dependent RNA polymerase enzymes which are necessary for the transcription and replication of viral genomes. The lack of research work and no compendial methods available for the estimation of this drug influenced the current research investigation to give a simple, sensitive, rapid, precise, accurate and robust isocratic high performance liquid chromatographic and UV Spectroscopic method for the determination and quantification of Favipiravir. The elution was done by using SHIMADZU Prominence-i, LC-2030 C system equipped with Shim-Pack GIST C18 (250X 4.6 mm, 5μm) column with a mobile phase mixture of 10 mM potassium dihydrogen ortho phosphate buffer (pH 4.0) and acetonitrile in the ratio of 90:10 v/v at a flow rate of 1.0 ml/min. The ultraviolet detection was done at the wavelength of 315 nm by maintaining column temperature at 30°. The total run time was 8.0 min. Calibration plot showed best regression over the concentration range of 10-60 μg/ml of Favipiravir standard solutions. The LOD and LOQ was found to be 0.18 μg/ml and 0.53 μg/ml, respectively. The accuracy of the proposed method was determined by performing recovery studies and was found to be between 99.47-100.80%. The repeatability testing for both sample and standard solutions was found as %RSD&lt;2.0% which is within the acceptable limits showing that the method is precise as well. The proposed method was successfully applied for the marketed formulations of Favipiravir tablets. In addition the main features of the proposed method are economic and eco-friendly with less retention time around 4.622 min.&#x0D;

GREEN SYNTHESIS OF SILVER NANOPARTICLES, METHOD DEVELOPMENT AND VALIDATION BY UV SPECTROSCOPY IN BULK PHARMACEUTICALS

The silver nanoparticle is an antibacterial, nontoxic agent. Its conventional synthesis usually generates toxic waste while reaction proceeds hence, green synthesis approach is used have for synthesis of silver nanoparticles (Ag-NPs) by using Datura metel leaf extract as reducing agent. The colour change from colourless to brown was the visual identification for formation of Ag-NPs and showed absorption at 447 nm. The Ag-NPs were of size 180 nm analysed by SEM and characterised by FTIR, where carboxylic peak was obtained at 1569 cm-1, besides confirming presence of alcoholic group and polyphenols. Further, validated method was developed and linearity was found to be 0.995 and % RSD of validation parameters was found to be within the limit &lt;2%. A simple, lab scale, rapid, accurate, precise and sensitive spectroscopic method has been developed and validated as per ICH guideline for synthesized Ag-NPs in bulk pharmaceuticals by UV vis spectrophotoscopy and it is applicable for routine analysis.

DEVELOPMENT AND VALIDATION OF UV-VISIBLE SPECTROPHOTOMETRIC METHOD FOR ESTIMATION OF TADALAFIL IN BULK AND FORMULATION

Objective: A new simple, sensitive, precise and reproducible spectroscopic method was developed for the determination of Tadalafil in Pharmaceutical formulation with Dimethyl Sulfoxide.&#x0D; Methods: The UV spectrum of Tadalafil in Dimethyl sulfoxide (DMSO) showed λ max at 285.6 nm. Beer’s law is valid in the concentration range of 10-60µg/ml. This method was validated for linearity, accuracy, precision, ruggedness and robustness.&#x0D; Results: The method was demonstrated excellent linearity over the range of 10-60µg/ml with regression equation y= 0.0337x-0.1343 and regression correlation R2= 0.998. Moreover, the method was found to be highly sensitive with LOD (2.44µg/ml) and LOQ (7.40µg/ml).&#x0D; Conclusion: Based on results, the proposed method can be successfully applied for assay of Tadalafil in various pharmaceutical dosage forms.

Oxidative Stress and Endothelial Dysfunction in the Development of Simulated Radio-Induced Lung Damage and their Correction with Pulmonary Surfactant

Radiation exposure to the chest organs used in the complex treatment of neoplasms is often accompanied by the development of radiation pneumonitis, fibrosis and respiratory failure.The aim of the study was to evaluate oxidative stress and endothelial dysfunction in radio-induced lung damage and possibility of their correction with a pulmonary surfactant preparation.Material and methods. Lung tissue samples of 82 male Wistar rats were investigated in the study. Single local irradiation of animals was performed with the X-ray RUM-17 unit at a dose 12 Gy. The quantitative content and fractional composition of phospholipids of pulmonary surfactant were determined in the study. Oxidative stress was detected using Raman spectroscopy, endothelial dysfunction was detected immunohistochemically.Results. Oxidative stress and endothelial dysfunction were registered starting from the first day of the experiment, and manifested by an increased content of free radicals and a decrease in endothelial function indices supported by precise spectroscopic, immunohistochemical and electron microscopic methods. With application of Surfactant-BL preparation oxidative stress manifestations were eliminated to the beginning of the intermediate stage of the experiment, and were preserved without correction until its completion.Conclusions. Three-fold intratracheal administration of a pulmonary surfactant preparation implements an antioxidant, immunomodulatory and compensating effect attenuating the alterative effect of oxidative stress and its initiating impact on the development of endothelial dysfunction. Native surfactant having a pronounced effect on all components of the lung tissue including alveolocytes of the first and second types and endothelial cells of the capillaries of the lung results in the correction of endothelial dysfunction.

UV spectrophotometric method development and validation of acotiamide in bulk and solid doage form

Objective: A new, simple, sensitive, precise and reproducible UV spectroscopic method was developed for the estimation of Acotiamide in bulk and Tablet Formulation. Methods: The UV spectrum of Acotiamide in water showed λ max at 249 nm. Beer's law is valid in the concentration range of 3–18μg/ml. This method was validated for linearity, accuracy, precision, ruggedness and robustness. Results: The method has demonstrated excellent linearity over the range of 3–18μg/ml with regression equation y = 0.0523x - 0.0429 and regression correlation coefficient r2= 0.9996. Moreover, the method was found to be highly sensitive with LOD (0.38μg/ml) and LOQ (1.17μg/ml). Conclusion: Depending on results the given method can be successfully applied for assay of Acotiamide in Tablet formulation.