Development Of Spectrophotometric Method Research Articles

Analytical Method Development and Validation of UV-Visible Spectrophotometric Method for the Estimation of Saxagliptin in Gastric Medium

Analytical Method Development and Validation of UV-Visible Spectrophotometric Method for the Estimation of Saxagliptin in Gastric Medium

Development and Validation of Ultra Visible Spectrophotometric Method for the Estimation of Thymoquinone

Aim: The work mainly focuses on developing a robust UV-Visible spectroscopic method for qualitative and quantitative analysis of thymoquinone and this will open to many possibilities in exploiting the wonders of this bioactive molecule.
 Study Design: UV-vis Spectrophotometric method development for thymoquinone.
 Place and Duration of Study: Department of Pharmaceutics, Department of Pharmaceutical Sciences, Rashtrasant Tukadoji Maharaj Nagpur University Campus, Nagpur, India.
 Methodology: To find out λmax and validate the developed method using Double beam UV – visible spectrophotometer module (JASCO V-630).
 Results: The thymoquinone was found to be soluble in methanol. The absorption maximum (λmax) was found to be 252 nm. The good linearity was found to be within concentration range of 2-10 μg/ml with correlation coefficient (r2) >0.99 and regression equation of the curve was found to be y = 0.0173x − 0.0394 at 252 nm. The precision (intra-day and inter-day) data represents good reproducibility with % RSD lower than 2.0% which assured that method is précised. Mean recovery value at different concentrations was found to be higher than 90%, indicates accuracy of the method. LOD and LOQ for thymoquinone were reported and were found to be 0.016 μg/ml and 0.0531μg/ ml 252 nm.
 Conclusion: The developed method was found to be simple, specific, economic, reliable, accurate, precise, and reproducible used as a quality control tool for analysis of pure thymoquinone and thymoquinone in formulations.

The Spectrophotometric Determination of Antiepileptic Drug in Standard and Pharmaceutical Formulations by Diazotization Coupling Reaction and Some Metals Complexes

A rapid, sensitive spectrophotometric method has been proposed for the determination of Gabapentin antiepileptic drug in pure and in pharmaceutical preparations was developed. The method is based on the coupling reaction between Gabapentin with8-hydroxy quinoline in to form an olive colored azo dye which gave maximum absorption at 365nm.The optimum reaction conditions like: pH, Temperature affected and time of reaction were evaluated. The ligand and its complexes were characterized by UV-visible spectroscopy, infrared FT-IR, (C.H.N.) analysis and Molar conductivity. The ratio of (metal: ligand) of all complexes was (1:2) by using molar ratio method and jop’s method. Beer’s law is obeyed for ligand and its complexes with (Cu2+, Ni2+,Cd2+, Co2+ and Zn2+) in concentration ranges ( 2 - 20, 1.5 - 25, 1 - 20, 2 - 25 and 2-30μg ml-) respectively . The molar absorptivity also calculated and it's found to be (1.396×104, 2.0208×104, 2.295×104, 1.684×104 and 1.862×104 L.mol-1.cm-1) for Cu2+, Ni2+,Cd2+, Co2+ and Zn2+complexes respectively. The detection of limit and quantification of limits are also calculated. The stability constant of complexes equal to(3.273×106, 1.695×102, 7.859×106, 1.851×105 and 1.588×102 L2.mol-2) for Cu2+, Ni2+,Cd2+, Co2+ and Zn2+ complexes respectively. The method is successfully used for the determination of Gabapentin in pharmaceutical formulations. Analytical parameters like accuracy and precision for the method have been established and evaluated statistically to assess the application of the proposed method. No interferes observed in the proposed method. The complexion with five ions (Cu2+, Ni2+, Cd2+, Co2+ and Zn2+) were studying. The aim of present work was devoted to investigate the reaction between Gabapentin and 8-hydroxy quinoline to form color Azo dye and use this product in the development of sensitive and simple spectrophotometric method for determination of Gabapentin in its pure and pharmaceutical preparations and spectrophotometric studies of a azo dye formed and it's metal complexes with Cu2+, Ni2+, Cd2+, Co2+ and Zn2+ ions.

Development of Green Spectrophotometric Method for Determination of Metoclopramide Hydrochloride

A simple, sensitive and green spectrophotometric method for the determination of metoclopramide hydrochloride (MTC) has been developed. The method is based on the reaction of MTC with p-dimethylaminobenzaldehyde (DAB) in acidic aqueous medium (pH 2) in the presence of anionic surfactant sodium dodecyl sulfate (SDS) to give a yellow colored Schiff’s base with a maximum absorbance at 452 nm. Obedience to Beer’s law is achieved in the concentration range 0.2–18.0 µg ml-1 (5.6×10-7 - 5.1×10-5 mol l-1), with relative error about 1%, relative standard deviation of less than 0.8% and molar absorptivity 3.02×10-4 l mol-1cm-1. The effect of the presence of some common pharmaceutical additives has been investigated. The developed procedure has been successfully applied to the determination of the drug in pharmaceutical formulations.

UV Spectrophotometric Method Development and Validation of Mesalazine in Bulk and Solid Dosage Form (Research Article)

UV Spectrophotometric Method Development and Validation of Mesalazine in Bulk and Solid Dosage Form (Research Article)

QUANTITATIVE ASSAY OF BINARY AND TERNARY CARDIOVASCULAR MIXTURES USING ABSORPTION SUBTRACTION SPECTROPHOTOMETRIC METHOD

Objective: Development and validation of specific spectrophotometric analytical method for the simultaneous determination of co-administered cardiovascular mixtures consisting of Aspirine (ASP) and Prasugrel (PRA) binary mixture and Ticagrelor (TICA), Irbesartan (IRB) and Hydrochlorothazide (HCT) ternary mixture.

Development of Spectrophotometric Method for Analysis of Framicetine Sulphate in a Medicinal Product and its Validation

A procedure for the quantitative determination of framycetin sulfate in the drug ‘Framex’ (nasal spray) 8000IU/ml has been developed, using spectrophotometry (SF) method. The developed method has been validatedusing the following indicators: specificity, correctness, linearity, repeatability and intralaboratory accuracy.It has been found that the developed methodology is valid for all characteristics and can be used for thequantitative determination of framycetin sulfate in the substances and composition of medicinal products.

Spectrophotometric method development and validation for simultaneous estimation of Anagliptin and Metformin HCl BY Q - Absorption ratio method in synthetic mixture

A simple, accurate, precise and economical Q- Absorption Ratio spectrophotometric method was developed and validated for estimation of Anagliptin and Metformin HCl in synthetic mixture. Anagliptin and Metformin HCl showed an iso-absorptive point at 238 nm in distilled water. The second wavelength used was 233 nm which is λmax of Metformin HCl in distilled water. The concentration of the drugs was determined by using ratio of absorbance at iso-absorptive point (λ1 = 238 nm) and at the λmax of Metformin HCl (λ2 = 233 nm). This method is linear for both drugs; in range of 2–12 μg/mL at λ1 (R2 = 0.999) and at λ2 (R2 = 0.9998) for Anagliptin, and in the range of 5–30 μg/mL for Metformin HCl found at λ1 (R2 = 0.9995) and at λ2 (R2 = 0.9997). The % Recovery was 100.42–101.83 % of Anagliptin and 99.94–101.63 % of Metformin HCl by standard addition method. The LOD was found to be 0.201 μg/mL and 0.262 μg/mL for Anagliptin at λ1 and λ2 respectively. The LOD was found to be 0.320 μg/mL and 0.167 μg/mL for Metformin HCl at λ1 and λ2 respectively. The LOQ was found to be 0.610 μg/mL and 0.794 μg/mL for Anagliptin at λ1 and λ2 respectively. The LOQ was found to be 0.972 μg/mL and 0.506 μg/mL for Metformin HCl at λ1 and λ2 respectively. The method was found to be precise as % RSD was less than 2.00 in Repeatability, Interday and Intraday precision for Anagliptin and Metformin HCl. The % assay of analyte drugs in synthetic mixture was found to be 100.601% of Anagliptin and 100.206 % of Metformin HCl which showed good applicability of the developed method.

Development of Indirect Spectrophotometric Method for Mercury Determination Based on The Formation of Iron(III)-Thiocyanate Complex

A new spectrophotometric method for mercury determination has been developed based on the complexation of mercury(II) in ascertained excess of thiocyanate. The remaining thiocyanate is reacted with iron(III) to form a red iron(III)-thiocyanate complex which gave maximum absorbance at 460 nm. The concentration of mercury(II) is inversely proportional to the decrease absorbance of the complex. The method was optimized to the concentrations of thiocyanate and iron(III). Selectivity of the method has also studied based on percent recovery of mercury(II) in the presence of common metal ions in the tailing waters of gold mine. Under the optimum conditions, the method showed linear correlation to mercury(II) concentration from 1-30 mg L−1 with detection limit of 0.58 mg L−1. The method was not interfered in the presence of all metal ions studied up to 50 mg L−1, except of silver which was tolerated at 10 mg L−1. The developed method has been satisfactorily applied for mercury(II) determination in synthetic and tailing waters of gold mine samples.

Analytical Method Development and Validation of First Order Derivative Spectrophotometric Method for Simultaneous Estimation of Telmisartan and Metformin Hydrochloride in their Combined Pharmaceutical Dosage Form

Ultra Violet (UV) Sectrophotomertic method has been developed for simultaneous estimation of telmisartan and metformin hydrochloride in bulk drug in their combined dosage form by first-order derivative. This method developed by using Methanol: Water (50: 50 v/v). Linearity was found near to 1, for telmisartan and Metformin hydrochloride. For Intraday, Interday, Intermediate precision, Robustness, %RSD was found less than 2. % Recovery was found to be between ranges 98-106% for both the drugs. These results indicate that the method is accurate, precise, and simple. All validation Parameter results comply with ICH guidelines.

Development and Validation for Simultaneous Estimation of Sofosbuvir and Daclatasvir Dihydrochloride in Pharmaceutical Dosage form by Ratio Derivative and Dual Wavelength Methods

Development and validation of new simple, sensitive, accurate and precise spectrophotometric method involving ratio derivative and dual-wavelength method, was done as per ICH Q2 (R1) for simultaneous estimation of Sofosbuvir (SOFO) and daclatasvir dihydrochloride (DACLA) in a combined dosage form. The overlapping in the spectra of both drugs was the reason for the selection of both methods. The absorbance difference (ΔA) value between 235.8 nm and 270.6 nm was selected for the quantitative determination of SOFO, where DACLA gives equal absorbance at the selected wavelength in the dual-wavelength method (Method A). The determination of DACLA is done quantitatively by measuring the difference in absorbance value at 249 nm and 268.6 nm where SOFO gives equal absorbance at a selected wavelength. Ratio spectra method (Method B) was based on dividing the spectra of a mixture with standard spectra of one of the analytes, and the first derivative spectra was recorded with Δλ = 8 nm and scaling factor 1. The amount of SOFO and DACLA was estimated in the binary mixtures by computing the first derivative signal at 247.0 nm and 341.0 nm, respectively. The calibration curve was linear in the concentration range of 10–90 μg/mL for SOFO and 4–20 μg/mL for DACLA for both the methods. The methods were successfully applied for the simultaneous determination of these drugs in combined dosage form with acceptable recoveries.

Development and Validation of Spectrophotometric Method for Propranolol Quantification in Capsule Formulation Containing Chitosan as Pharmaceutical Excipient

The use of chitosan as a diluent in propranolol capsules was evaluated, where its performance was compared with that of microcrystalline cellulose. A spectrophotometric method was validated to quantify propranolol in these capsules, where weight variation, drug content and dissolution were evaluated. The quantification of propranolol was carried out at 290 nm in the range of 32–48 mg/L. The specificity, linearity, limits of detection and quantification, precision, accuracy and robustness of this method were in accordance with regulatory parameters. Propranolol capsules prepared using both diluents exhibited weight variations and drug contents within acceptable limits. The dissolution studies showed that the use of chitosan as a diluent is a promising alternative to capsules for modulation of water soluble drugs release, such as propranolol. The present study reveals an alternative approach of higher functionality of chitosan as a diluent in solid dosage forms when compared to a traditional diluent – microcrystalline cellulose.

Spectrophotometric method Development and validation of Acotiamide in its bulk and Tablet Dosages Form.

Spectrophotometric method Development and validation of Acotiamide in its bulk and Tablet Dosages Form.

Development of a new visible Spectrophotometric analytical method for determination of Vildagliptin in bulk and Pharmaceutical dosage forms

Development of a new visible Spectrophotometric analytical method for determination of Vildagliptin in bulk and Pharmaceutical dosage forms

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.

Development and Validation of Spectrophotometric and Chromatographic Method for the Estimation of Apremilast in Bulk and Formulations

Objective: Objective of the present analytical research work was to develop and validate Spectrophotometric method and High Performance Liquid Chromatographic method (HPLC Method) for the Apremilast bulk and tablets dosage form.
 Methods: A spectrophotometric method and a HPLC method have been developed and validated for estimation of APR in pharmaceutical oral dosage form.
 Method A (UV SPECTROMETRY Method): The stock and working standard solutions of the drugs were prepared in methanol. Standard solutions were scanned over the range of 400-200 nm in spectrum mode of spectrophotometer at medium scanning speed using UV spectrophotometer. The maximum absorbance for Apremilast was found at 230 nm.
 Method B (HPLC Method): The HPLC Method for Apremilast was developed using Cosmosil C18 (4.6mm x 250mm, Particle size: 5µm), as stationary particle, isocratic mode. Methanol: Water (80:20v/v) pH3 as mobile phase. Mobile phase was maintained at a flow rate of 0.8 ml/min and detection was carried out at 230 nm. Both the methods were validated in accordance with ICH guidelines
 Results: Apremilast was found to be linear in the concentration range of 2-10 µg/ml for spectrophotometric method and 10-50 µg/ml for HPLC method. Retention time was found to be 4.0 min for Apremilast. The amount of Apremilast in marketed formulation by spectrophotometric method was found to be 99.82 %, the amount of Apremilast in marketed formulation by HPLC method was found to be 99.98 %.
 Interpretation and Conclusion: Results of assay and validation study were found to be satisfactory. So, the methods can be successfully applied for the routine analysis of Apremilast.
 Keywords: HPLC, bulk dosage form, tablets,

Comparative dissolution studies on granules with acetaminophen and caffeine using the basket and paddle methods with simultaneous spectrophotometric determination of active substances

Abstract Acetaminophen and caffeine, popular therapeutic substances used to relieve pain or alleviate the symptoms of cold. The aims of the study were the comparison of granules, in terms of dissolution rate and moreover the development of spectrophotometric method to the simultaneous determination of both active pharmaceutical ingredients (APIs) in granules. The granules were tested by two pharmacopoeial methods of dissolution for solid dosage forms, and the dissolution profiles for each formulation were compared. A method of simultaneous determination of two medicinal substances by the double calibration method using derivative spectrophotometry was used. Considering the dissolution process carried out in the paddle apparatus, it was shown that more than 80% of acetaminophen and caffeine were released from each of the preparations in a clearly shorter time than 10 minutes. Carrying out the basket test, substances dissolved gradually, much slower than in the paddle method. The time required to release 80% of both active substances from majority of tested preparations was from 30 to 45 minutes. Application of the first derivative spectrophotometric method allows simultaneous determination of acetaminophen and caffeine in the mixture, without the need to separate them first.

Spectrophotometric Method Development and Validation for Simultaneous Estimation of Nebivolol hydrochloride and Valsartan in Bulk and Combined Pharmaceutical Dosage Form in Release Media

A simple, rapid, precise, accurate and sensitive spectrophotometric method has been developed for the simultaneous estimation and validation of Nebivolol Hydrochloride (NEB) and Valsartan (VAL) in pure and combined tablet dosage forms. Pure drug samples of NEB and VAL were dissolved in 67 mM Phosphate buffer pH 6.8 with 0.5 % sodium dodecyl sulphate (SDS) and found to have absorbance maxima at 280 nm for NEB and 250 nm for VAL, respectively. The linearity lies between 10-70 μg/ml for NEB and 10-60 μg/ml for VAL in this method. The correlation coefficient (r2) was found to be 0.9965 for NEB and 0.9960 for VAL. The % recoveries obtained were 95.65 % – 109.85 % for NEB and 97.42 % – 101.43 % for VAL. The % RSD found 0.271 %-1.490 % for intraday and 0.334 %-1.917 % for interday for NEB and 0.188 %-0.944 % for intraday and 0.392 %-1.197 % for interday for VAL. The limit of detection and limit of quantitation for NEB were found to be 4.608 μg/ml and 13.965 μg/ml respectively and the limit of detection and limit of quantitation for VAL were found to be 4.348 μg/ml and 13.178 μg/ml respectively. Simultaneous calibration of both drugs in 67 mM Phosphate buffer pH 6.8 with 0.5 % SDS shows that λmax of one drug does not interfere on the λmax of other drug. Recovery study was performed to confirm the accuracy of the method. The results of analysis have been validated statistically by recovery studies as per International Conference on Harmonization guidelines. The method showed good reproducibility and recovery with % RSD <2. Hence, this proposed method was found to be rapid, specific, precise, accurate and can be successfully applied for the routine analysis of NEB and VAL in pure and combined tablet dosage form.

Isolation of mitraphylline from Uncaria tomentosa (Willd. ex Schult.) DC. barks and development of spectrophotometric method for total alkaloids determination in Cat's Claw samples.

AbstractIntroductionThe usual quality control for Uncaria tomentosa (Willd. ex Schult.) DC. barks requires highly specific analytical standards and methods based on high‐performance liquid chromatography (HPLC), which impacts the costs of the analytical process and the final products.ObjectiveTo obtain an analytical reference standard of mitraphylline by isolation from U. tomentosa barks and develop a spectrophotometric method for determination of total alkaloids in samples of U. tomentosa.MethodologyAn alkaloid‐enriched extract was obtained by acid–base partition and mitraphylline was selectively precipitated using an 80:20 v/v toluene/hexane solution. The compound was characterised by HPLC‐UV/DAD (diode‐array detector), mass spectrometry, UV‐visible, infrared (IR) and 1H‐ and 13C‐nuclear magnetic resonance (NMR) spectroscopy. Sample preparation for the spectrophotometric method consisted of an extraction with boiling methanol (3 × 10 mL, 15 min), followed by a strong cation exchange solid phase extraction (SCX‐SPE) clean‐up.ResultsMitraphylline with a purity of 98% was isolated in 0.05% m/m yield. All characterisation results were in agreement with previous published data. The spectrophotometric method showed linear range between 0.40 and 20 μg/mL; limits of detection and quantification of 0.15 and 0.49 μg/mg, respectively; dispersion of results lower than 5% for repeatability and intermediate precision; statistically proven accuracy by comparison with reference values obtained by Soxhlet and an HPLC‐UV/DAD method; and robustness in relation to sample mass extracted and extraction time.ConclusionThe methods developed to obtain mitraphylline analytical standard from U. tomentosa barks and to determine total alkaloids by spectrophotometry provided a cheaper and faster quality control alternative for U. tomentosa samples.

New Derivatization Methodology of 4-aminobenzoic Acid from its Dietary Supplements: Kinetic Spectrophotometric Methods for Determination

Background:A new approach describing the validation and development of an easy, new spectrophotometric and kinetic method for identification of para-aminobenzoic acid in dietary supplement has been performed. In this study, para-aminobenzoic acid was derived in a pH-controlled environment, as a new organic compound 4(4-Benzophenylazo)pyrogallol, by incorporating diazotized para-aminobenzoic acid with pyrogallol.Objective:The determination of para-aminobenzoic acid was conducted by the fixed time and initial rate techniques. These approaches were based on the reaction of the compound containing paraaminobenzoic acid, 4(4-Benzophenylazo)pyrogallol, with Ag(I) to form colored product with a maximum absorbance at 468nm. Both of these techniques were adopted for constructing the calibration curves and examined for their suitability for the quantitation of para-aminobenzoic acid in dietary supplement.Methods:The determination process was established, using initial rate and fixed time kinetic spectrophotometric methods.Results:4(4-Benzophenylazo)pyrogallol was characterized using proton-nuclear magnetic resonance, Fourier-transform infrared, differential scanning calorimetry and thermogravimetric thermal methods, gas chromatography–mass techniques, and solvatochromic behavior in solvents with different polarities was also examined.Conclusion:For the first time, para-aminobenzoic acid was well determined by incorporating it as an organic solid compound, 4(4-Benzophenylazo)pyrogallol, through coupling pyrogallol with diazotized para-aminobenzoic acid in regulated pH medium, ranging between 5.0 to 6.0. The existence of common excipients in the dietary supplement did not produce any significant interference. F- and ttest data analysis were used for statistical comparison of the suggested techniques with that of reference method, demonstrating excellent agreement with no significant difference in the associated precision and accuracy.