Spectrophotometric Method For Simultaneous Estimation Research Articles

Development and Validation of UV Spectrophotometric Method for Simultaneous Estimation of some SGLT-2 and DPP-4 inhibitor in Bulk and Pharmaceutical Dosage Form

The result of pharmaceutical industry research for the new class and the new combination of drugs for the treatments of diabetes is the newly approved combination of Remogliflozin etabonate (RGE) and Teneligliptin Hydrobromide hydrate (TG). For the quality control of this formulation, the smart, reproducible and non-sophisticated spectroscopic techniques were developed by modification of UV spectra. The proposed methods exhibited Beer’s law in the range of 10 to 60µg/ml and 5 to 30µg/ml for RGE and TG correspondingly. The mean percentage recovery was found to be in the range of 98.60 to 101.55 for RGE and 99.87 to 100.21 for TG. Further, both analytes were quantified from the formulation using proposed spectroscopic methods with high accuracy. The suggested technique is simple, accurate and reproducible, hence could be used for regular quality control of formulation consisting of RGE and TG. The developed method can be used for analysis of stability samples and routing quality control evaluation in tablet formulation.

Development and Validation of FT-IR Spectrophotometric Method for Simultaneous Estimation of Clonidine Hydrochloride and Chlorthalidone in Pharmaceutical Synthetic Mixture

A precise, simple, cost effective, accurate, eco-friendly and validated fourier transform infrared spectroscopy method has been developed for the simultaneous estimation of Clonidine Hydrochloride and Chlorthalidone in pharmaceutical synthetic mixture. The developed method involves measurement of spectral wavenumber of the infrared band corresponding to (–C=N) from 1658.78 cm-1 for Clonidine Hydrochloride and (-S=O) group from 1346.31 cm-1 for Chlorthalidone. Over the range of 1.5–3% w/w for Clonidine hydrochloride and 15–90% w/w for Chlorthalidone, the method was found to be linear. It has correlation coefficient (r2) of 0.999 for Clonidine hydrochloride and 0.994 for Chlorthalidone. According to ICH guidelines, in terms of accuracy, linearity, limit of detection and limit of quantitation, precision, the developed method was validated. In addition to this, degradation behaviours of Clonidine Hydrochloride and Chlorthalidone were studied by subjecting them to sunlight, photolytic and thermal degradation.

Evaluation of Stability and TLC Fingerprinting of the Artemether Component in Artemether-Lumefantrine Combination Suspension Formulations Available in Nigeria Pharmaceutical Market

Aim: Artemether is the main component of the artemisinin-based combination therapy (ACT), used in the management of malaria infection caused by Plasmodium falciparum. Hence, its stability and conformation to pharmacopeia standards are necessary for use. The study aimed to review the first-order derivative spectrophotometric method for simultaneous estimation of artemether and its derivatives in pure and combined formulations, and their stability profiles, then develop a simple, precise, and fast technique for their rapid physicochemical analysis.
 Methodology: Thin-layer chromatographic (TLC) Fingerprinting principles were used in the analysis. Artemether and its derivatives were spotted on the TLC chromatograms after adding 25 mL of the suspension to a mixture of 100 mL of distilled water and 4 mL of NaOH, extracting the mixture with 60 mL of dichloromethane (DCM), drying, and sonicating the residue with 20 mL of the solvent. It was centrifuged, and the clear supernatant was spotted on the TLC plates.
 Results: The color test results revealed the presence of the artemether compound in the reference standard as well as the six brands of suspensions (A, B, C, D, E, and F) utilized in the study. Artemether melting point was obtained between 86 - 89 °C; within the International Pharmacopeia specified range. The chromatograms of Artemether and derivatives showed Rf values of 0.25 (impurity A), 0.3 (artenimol impurity B), 0.35 (impurity C), 0.4 (α-artemether: impurity D), and 0.55 (artemether).
 Conclusion: The devised method can be applied to the routine quality control analysis of artemether-lumefantrine suspension in addition to existing analytical techniques.

Development and Validation of Stability Indicating UV Spectrophotometric Method for Simultaneous Estimation of Indacaterol and Momestasone Furoate in Pharmaceutical Dosage Form

A simple, accurateand precise stability indicating UV spectrophotometric method has been developed for simultaneous estimation of Indacaterol and Momestasone Furoate in pharmaceutical dosage form. The absorbance of Indacaterol and Momestasone Furoate was measured at two different wavelength 260 nm and 224 nm. It shows linear response between the concentration ranges 12-18 µg/ml and 25.6-38.4 µg/ml of regression coefficient r2 being 0.9994 and 0.9994 of Indacaterol and Momestasone Furoate, respectively. A recovery study was carried out to confirm the methods accuracy. In the recovery study, the % RSD was less than 2. The % degradation by acidic, basic, oxidation, thermal and photolytic degradation of Indacaterol was found to be 5.39, 2.37,3.46, 2.43 and 1.64%, while of Momestasone Furoate it was 2.37, 11.44, 1.18, 9.88 and 2.35%.The method for estimation of Indacaterol and Momestasone Furoate was found to be precise, specific, reproducible & economical, as per ICH guideline the results of analysis were validated and found to be satisfactory.

Development and Validation by UV Spectrophotometric Method for Simultaneous Estimation of Gliclazide and Quercetin in Formulation

Abstract: A simple, quick, accurate, precise, and cost-effective spectrophotometric approach for simultaneous estimation of Gliclazide and Quercetin has been developed by Simultaneous equation method. Gliclazide and Quercetin shows absorbance maximum at 226 and 255 nm respectively, as a result absorbance was measured at these wavelengths for the estimation of Gliclazide and Quercetin. In concentration ranges from 2-18 g/ml, and 2-22 g/ml for Gliclazide and Quercetin respectively followed Beer-Lambert's law. The method has been developed and validated in accordance with ICH recommendations and can be used for estimation of Gliclazide and Quercetin in formulations.

Development and Validation by UV Spectrophotometric method for Simultaneous Estimation of Fluconazole and Thymol in Formulation

Abstract: Simultaneous equation technique has devised a simple, rapid, accurate, precise, and cost-effective spectrophotometric strategy for simultaneous estimation of Fluconazole and Thymol. Fluconazole and Thymol had absorbance maxima at 261 and 273 nm, respectively; hence absorbance was measured at these wavelengths for fluconazole and Thymol estimate. Fluconazole and Thymol followed Beer-Lambert's rule in concentration ranges of 20-140 g/ml and 20-100 g/ml, respectively. The technique was developed and verified in compliance with ICH guidelines and may be used to estimate Fluconazole and Thymol concentrations within formulations.

Second-Order Derivative Spectrophotometric Method for Simultaneous Estimation of Azilsartan Medoxomil and Cilnidipine in Combined Dosage Form

Second-Order Derivative Spectrophotometric Method for Simultaneous Estimation of Azilsartan Medoxomil and Cilnidipine in Combined Dosage Form

Development of spectrophotometric method for simultaneous estimation of dexketoprofen and dicyclomine

Objectives: The objective of this work was to develop a simple, fast, and reliable ultraviolet (UV) spectrophotometric method for simultaneous estimation of dexketoprofen and dicyclomine in tablet dosage forms. Materials and Methods: Dexketoprofen and dicyclomine solutions were prepared separately in the range of 2 µg/mL–10 µg/mL. The solutions were scanned over a range of 200–400 nm. The isoabsorptive point for both drugs was determined. The developed method was evaluated for accuracy, precision, and linearity. In linearity correlation coefficient was found. Results: A simple, fast, and reliable UV spectrophotometric method was developed for quantitative estimation of dexketoprofen and dicyclomine. The precision study showed that the percent relative standard deviation was within the range of acceptable limits, and the percent recovery was found to be in the range of 0.3–1.5 (intraday) and 0.23–1.7 (interday). In the accuracy study, the percent recovery was found to be 97 (50%), 96 (100%), and 95 (150%). Conclusion: The developed spectrophotometric method in this study was simple, accurate, precise, specific, sensitive, and reproducible and can be directly and easily applied to pharmaceutical dosage forms.

Development and validation of Q-absorbance ratio spectrophotometric method for simultaneous estimation of ondansetron HCl and esomeprazole magnesium in bulk and formulation

Development and validation of Q-absorbance ratio spectrophotometric method for simultaneous estimation of ondansetron HCl and esomeprazole magnesium in bulk and formulation

Development of UV- Spectrophotometric Method for Simultaneous Estimation of Metformin and Piperine in Combined Tablet Dosage Form

Piperine is an alkaloid obtained from Piper nigrum Linn., is known to modify the biotransformation of the drugs by inhibiting Cytochrome P450 forms. Piperine inhibits the bio-transformation and metabolism of metformin leading to higher levels of drug in systemic circulation, thus increases the bioavailabilty when co-administered with metformin. In the present study a simple, accurate, precise, economical procedures, entailing neither irksome sample treatment nor tedious extraction process a combined tablet dosage form of metformin and piperine have been developed for the simultaneous estimation of piperine and metformin using UV- Spectrophotometry method. The developed method was based on employing simultaneous equation method for analysis of both the drugs. Metformin and piperine have shown absorbance maxima at 237nm and 342nm respectively, in methanol and the linearity was obeyed over the concentration range of 2-10μg/ml and 2-10 μg/ml respectively for metformin and piperine. The validation parameters like precision, accuracy, limit of quantitation (LOQ), limit of detection (LOD), were determined according to ICH guidelines. All the results were found to be within the limits.

Stability Indicating RP-HPLC and Spectrophotometric Methods for Simultaneous Estimation of Sodium Benzoate and Cefdinir in the Presence of its Degradation Products-Application to Blank Subtraction Method.

Empower 3 software is important in modeling, optimization, and reducing the time of manual calculation of related substance by subtracting the baseline of a blank chromatogram from the unknown sample automatically; so, the major objective of the developed method is to introduce a new, selective, and economical high performance liquid chromatography (HPLC) and spectrophotometric method for simultaneous estimation of sodium benzoate (SDB) and cefdinir (CFR) in the presence of its degradation products. Chromatographic separation is optimized and adjusted using two methods; method (I) is characterized for separation of active pharmaceutical ingredient (CFR) in pure and dosage forms using Atlantis dC18 column [4.6 mm x 250 mm (5 μm particle size or equivalent)] with a mobile phase consisting of methanol: 0.02 M phosphate buffer solution pH 3.0 (40:60 v/v) at a flow rate of 1.0 mL/minute, injection volume 10 μL and wavelength 254 nm. Method (II) is identified for related substances in a Hichrom C18 column (15 x 0.46 cm), 5 μm particle size or equivalent, using a binary gradient consisting of solution A [0.1% tetramethylammonium hydroxide solution (pH: 5.5) with 0.1 M EDTA (1000:0.4 v/v)] and solution B (0.1% tetramethylammonium hydroxide solution (pH 5.5): acetonitrile: methanol : 0.1 M EDTA (500:300:200:0.4 v/v) using injection volume 10 μL for reversed-phase HPLC with a wavelength equals to 254 nm and flow rate 1.0 mL/min. Two ecofriendly spectrophotometric methods were successfully used to resolve the spectral overlap of drugs. Method A, the first derivative of ratio spectra spectrophotometric method (1stDD) where CFR was determined at two wavelengths 283.5 nm, 313.4 nm and SDB was determined at 216.7 nm, 235.5 nm. Method B, ratio subtraction method is performed to overcome the interference between CFR and the preservative SDB. The ultraviolet spectrum of the laboratory mixture is divided by that of CFR (20 μg/mL) as a divisor then subtracting the amplitudes in the plateau region at 250-315 nm (the constant) from that of the ratio spectrum. The zero-order spectra of SDB were obtained at 225 nm by multiplying the resulting ratio spectra by the divisor (CFR), zero order of CFR was been estimated at a wavelength value of 283 nm after multiplication of the divisor by the obtained constant. The optimized method was adjusted and validated as per International Conference on Harmonization guidelines and could be easily utilized by quality control laboratories and for laboratory-prepared mixtures.

Development and Validation of UV Spectrophotometric Methods for Simultaneous Estimation of Dolutegravir Sodium and Rilpivirine Hydrochloride in Pure Bulk Form

A simple, specific, sensitive, rapid, precise, accurate and economical UV Spectrophotometric simultaneous equation method have been developed and validated for the routine estimation of Dolutegravir sodium and Rilpivirine Hydrochloride in bulk form. The Method A employs estimation of drugs by simultaneous equation method (SEM) using synthetic mixture of drugs. The absorption maxima of drugs were found to be at 259.20nm for Dolutegravir sodium and 305.80nm for Rilpivirine Hydrochloride. Both drugs followed the beer lamberts law in the range of 4-24µg/ml and 1-8µg/ml for DOL and RIL respectively. Methods are validated according to ICH guidelines and can be adopted for the routine analysis Dolutegravir sodium and Rilpivirine Hydrochloride in pure bulk form.

Eco-Friendly UV Spectrophotometric Method for Simultaneous Estimation of Evogliptin and Metformin Hydrochloride in Bulk and Combined Tablet Dosage Form

Evogliptin (EGT) is used in fixed-dose combination with metformin hydrochloride (MFH) for a better glycemic control in Type 2 diabetes mellitus. To date, no method is available for simultaneous estimation of these drugs. In the present study, an UV spectrophotometric method was developed in distilled water, an environment-friendly solvent using the simultaneous equation technique to simultaneously determine EGT and MFH in bulk and tablet dosage form. The developed method was validated and applied to commercial tablet dosage forms containing EGT and MFH in combination. With a great correlation value (R2>0.998), the analytes displayed good linearity in the range of 10-100 μg mL-1. The low percent relative standard deviation proved the methods' precision. The methods' accuracy was demonstrated by excellent recovery. Thus, the developed method was found to be simple, environment-friendly, fast, specific, precise, and accurate, and it may be effectively used for routine analysis of EGT and MFH in bulk and their combined tablet dosage form.

Development and validation of UV Spectrophotometric method for simultaneous estimation of Efonidipine hydrochloride ethanolate and Chlorthalidone in their synthetic mixture

Efonidipine Hydrochloride Ethanolate and Chlorthalidone is used in management of hypertension and under clinical phase 3 study. The development of quality control method is required for accurate analysis of both drugs. Two simple, precise and economical UV spectrophotometric methods have been developed for the simultaneous estimation of Efonidipine Hydrochloride Ethanolate and Chlorthalidone in their synthetic mixture. Method I is simultaneous equation method (Vierodt’s Method), which is based on measurement of absorption at 251 and 227 nm i.e. λmax of Efonidipine Hydrochloride Ethanolate and Chlorthalidone, respectively. Method II is first order derivative was based on the measurement of absorbance of Efonidipine Hydrochloride Ethanolate measure at 283.2 nm (ZCP of Chlorthalidone) and absorbance of Chlorthalidone measure at 250.8 nm (ZCP of Efonidipine Hydrochloride Ethanolate). Linearity was observed in the concentration range of 6.4-38.4 µg.mL-1 for Efonidipine hydrochloride ethanolate and 2-12 µg.mL-1 for Chlorthalidone using methanol as a solvent. The accuracy of methods was assessed by recovery studies and was found to be within range of 98-102% for both the drugs. Precision of the methods was estimated by repeatability and intermediate precision studies. The % RSD values were found to be less than 2, proving methods were precise. Two methods were compared using F- test. The results were validated statistically as per ICH Q2 R1 guideline and were found to be satisfactory.

Development of a UV visible spectrophotometric method for simultaneous estimation of Ranolazine and Metoprolol

Ranolazine being Na+ channel blocker agent, decreases the chances of angina attacks. Metoprolol exerts specific β1 blocking effect which results into decreased cardiac contractility and heart Rate (1). Ultimately reduces oxygen demand of heart. Metoprolol enhances the pharmacological activity of Ranolazine so the combination gives better therapeutic activity (2).
 There is no UV visible method present for the simultaneous estimation of Ranolazine and Metoprolol. To formulate and evaluate such a formulation involving mentioned drugs this simultaneous equation method was developed using 0.1 N HCl as a solvent. Chosen wavelengths were 272 nm and 242 nm for Ranolazine and Metoprolol Succinate respectively. Linearity range was seen to be 7.5 to 40 ppm for Ranolazine and 1 to 5 ppm for Metoprolol. Recovery studies and Validation were successfully performed according to ICH guidelines. This method can be applied for any formulation consisting mentioned drugs without interference of other excipients.
 Keywords: UV visible spectrophotometry, Simultaneous estimation, Ranolazine, Metoprolol succinate, Analytical Method development, Angina Pectoris

Development and Validation of a Novel, Cost Effective UV Spectrophotometric Method for Simultaneous Estimation of Cilnidipine and Olmesartan

Cilnidipine is a novel, dihydropyridine class of calcium-channel blocker. It prevents intracellular calcium influx and results in vasodilatation. Olmesartan medoxomil is a synthetic imidazole derivative prodrug and angiotensin II type blocker used to manage hypertension. The combination of cilnidipine and olmesartan medoxomil is used in the treatment of hypertension. Literature review revealed that there are many analytical methods involving HPLC and some using UV for estimation of the two drugs individually and in combination. UV spectrophotometric methods have the advantage of being simple, cost effective and rapid. Hence it was thought worthwhile to develop a simple, cost effective UV spectrophotometric method for simultaneous estimation of cilnidipine and olmesartan medoxomil employing the Absorption Correction principle. In this method, water: methanol (80:20,v/v) was used as the diluent. From the UV overlain spectra of both the drugs 257nm and 365nm were selected as wavelengths for analysis. The method was validated using the ICH guidelines. The linearity range was established from 10-100µg/ml (r2= 0.999) for cilnidipine and 10-80 µg/ml (r2= 0.998) for olmesartan medoxomil. The developed method was found to be accurate as % recovery at 80%, 100% and 120% levels were found to be within the acceptance criteria. The results for intra-day and inter-day precision were within acceptance limits of % RSD ˂ 2%. The method was found to be sensitive and robust. The developed method was applied in the estimation of Cilnidipine and Olmesartan in tablet dosage form and % assay was found to be 100.75% and 103.8% for the two drugs respectively. Hence the developed method can be employed as a simple, cost effective, quality control analytical method for simultaneous estimation of the two drugs in bulk and in combination.

Development and Validation of Spectrophotometric Methods for Simultaneous Estimation of Cefixime Trihydrate and Linezolid in Tablet Dosage Form

A new, simple, rapid and novel spectrophotometric method has been developed for simultaneous estimation of cefixime trihydrate and linezolid. For this, simultaneous equation method is used. The method involved measurement of absorbance at two wavelengths, 250 nm and 286 nm, λ max of linezolid and cefixime trihydrate respectively. This method obeys Beer’s law in the employed concentration ranges of 2-12 μg/ml for both cefixime trihydrateand linezolid. The proposed method is recommended for routine analysis since it is rapid, simple, accurate, specific and also sensitive. This paper describes the development and validation of UV spectroscopic method for simultaneous estimation of cefixime trihydrate and linezolid in Tablet dosage form.

Development and Validation of Difference Spectrophotometric Method for Simultaneous Estimation of Rosuvastatin Calcium and Aspirin in Marketed Formulation

Objective: To develop and validate a simple Vierordt method for the simultaneous estimation of rosuvastatin calcium (RSV ca) and aspirin (ASP) in fixed dose combination capsules by difference spectrophotometry technique in the UV region. Difference spectrophotometry is based on the utilization of difference absorption spectra corresponding to the same compound obtained at two different pH values. 
 Methodology: The difference in spectral characteristics for the two drugs was observed in 0.01N acetic acid and 0.01N NaOH. The simultaneous equations were developed using difference absorbance and absorptivity values of the two drugs measured and calculated at 243.2nm and 297nm for RSV ca and ASP respectively.
 Results: Two drugs have shown very good linearity in the concentration range of 10-100µg/ml. The methods were validated as per ICH guidelines for the limit of detection, the limit of quantification, accuracy, and precision, which were found to be within the acceptable limits. The validated method was successfully applied for the analysis of rosuvastatin calcium and aspirin in fixed dose combination capsules.
 Conclusion: Because this approach is simple and does not require a particular programme, it can be used as a substitute for LC methods in quality control laboratories that lack the necessary equipment for those techniques.
 
 

Four chemometric spectrophotometric methods for simultaneous estimation of amlodipine besylate and olmesartan medoxomil in their combined dosage form

For determination of amlodipine besylate (AML) and olmesartan medoxomil (OLM) at the same time, four UV chemometric spectrophotometric techniques were created and tested in accordance with ICH standards. Method (I) was absorption subtraction method (ASM) using two wavelengths, one of which was of AML at 365 nm and the other was the isoabsorptive point of both drugs at 237 nm. Method (II) was ratio subtraction method (RSM) for determination of OLM at λmax = 254 nm by taking the ratio spectrum and subtracting the constant values using 10 μg/mL of AML as a divisor in combination with extended ratio subtraction method (ERSM) to determine AML at λmax = 239 nm using 10 μg/mL OLM as a divisor. Method (III) was dual wavelength method; the wavelengths used to determine OLM were 221 nm and 235 nm, while those used to determine AML were 246 nm and 259 nm. Method (IV) was the second order derivative (2D) spectrophotometric method at 219 nm for OLM and 227 nm for AML. The proposed approaches were used to achieve linearity in the concentration range of 2–25 μg/mL for both drugs. The approaches were found to be uncomplicated, reproducible, efficient, and cost-effective as well as they were successfully used to determine the cited drugs in both laboratory samples and commercial pharmaceutical formulations.

Ecofriendly Simple UV Spectrophotometric and Chemometric Methods for Simultaneous Estimation of Paracetamol Aceclofenac and Eperisone Hydrochloride in Pharmaceutical Formulation: Assessment of Greenness Profile

This work introduces three eco-friendly UV spectrophotometric methods for the simultaneous estimation of Paracetamol, Aceclofenac and Eperisone Hydrochloride in pharmaceutical tablet formulation. The procedures employed were simultaneous equation method and multivariate chemometric methods with phosphate buffer pH 7.80 as diluent. The simultaneous equation method encompasses absorbance measurement at three different wavelengths (λmax of the drugs). It exhibits linearity between 12–18 µg mL−1 for paracetamol, 3.69–5.53 µg mL−1 for Aceclofenac, and 2.76–4.15 µg mL−1 Eperisone hydrochloride. The results obtained for accuracy and precision by the simultaneous equation method were within the permissible limits. Principal component regression and partial least squares were the tools used for chemometric methods. The calibration set and prediction set were constructed, and the UV spectra were recorded in zero order mode, further subjected to chemometric analysis. The % recoveries obtained for Paracetamol, Aceclofenac, and Eperisone Hydrochloride by chemometric techniques showed good accuracy, and the results obtained for analytical figures of merit were acceptable. Statistical comparison of the assay results obtained for the proposed methods showed no significant difference found among the methods using one way analysis of variance. Greenness evaluation tools revealed the greenness profile of the proposed methods and found them to be ecofriendly. The described methods were appropriate for routine quality control laboratories, facilitating eco-friendly, fast, and cost effective determination of Paracetamol, Aceclofenac, and Eperisone Hydrochloride in Acemyoset P tablets.