Validation of simultaneous volumetric and spectrophotometric methods for the determination of captopril in pharmaceutical formulations

Simple, sensitive and economical simultaneous volumetric and spectrophotometric methods for the determination of captopril have been developed. The methods were based on the reaction of captopril with potassium iodate in HCl medium. Amaranth was used as indicator to detect the end-point of the titration in aqueous layer. The iodine formed during the titration was extracted into CCl4 and subsequently determined spectrophotometrically at 510 nm. The Beer's law was obeyed in the concentration range of 120-520 microg ml-1. Rigorous statistical analyses were performed for the validation of the proposed methods. The proposed methods were successfully applied to the determination of captopril in dosage forms. Comparison of the means of the proposed procedures with those of reference methods using point and interval hypothesis tests showed no statistically significant difference.     

A rapid and selective solid-phase UV spectrophotometric method for determination of ascorbic acid in pharmaceutical preparations and urine

Ascorbic acid was determined by a solid-phase UV spectrophotometry technique through the sorption of this on a dextran-type anion-exchange resin, Sephadex QAE A-25 and posterior direct measurement of its absorbance on the resin at 267 and 400 nm, packed in a 1-mm cell. The calibration graph was linear over the range 0.3-5.0 microg ml(-1). The sensitivity obtained is more than 50 times higher than that of the corresponding solution method. The detection limit was 0.05 microg ml(-1) and the relative standard deviation 0.74% (n = 10). This method is very rapid and highly selective for determining ascorbic acid in the presence of other species absorbing in the ultraviolet region and which are normally encountered with it. The one-step method proposed was successfully applied in the determination of ascorbic acid in pharmaceutical preparations and urine and the results were of comparable accuracy as indicated by a statistical analysis of the data, using both t- and F-tests.     

Direct spectrophotometric determination of quercetin in the presence of ascorbic acid

The current research provides a simplified sample preparation procedure for the accurate estimation of quercetin in pure and in the pharmaceutical dosage form. Direct spectrophotometric method for the determination of quercetin in the presence of ascorbic acid was established. The influences of medium, wavelength, pH, temperature and the ionic strengths on quercetin determination were investigated. The best conditions for calibration curve are: 50% ethanol, lambda = 370 nm, pH = 4.2, T = 34 degrees C and I = 7.5 x 10(-5) M. Beer's law is obeyed in the concentration range 1.0-12.0 microg ml(-1) for quercetin. The corresponding detection limit is 0.76 microg ml(-1). The proposed method was verified by analyzing Quercetin + C capsules, Twinlab.     

Sensitive kinetic spectrophotometric determination of captopril and ethamsylate in pharmaceutical preparations and biological fluids

A highly sensitive kinetic spectrophotometric method was developed for the determination of captopril (CPL) and ethamsylate (ESL) in pharmaceutical preparations and biological fluids. The method is based on a catalytic acceleration of the reaction between sodium azide and iodine in an aqueous solution. Concentration range of 0.1-1.5 microg ml(-1) for CPL and 0.3-3 microg ml(-1) for ESL was determined by measuring the decrease in the absorbance of iodine at 348 nm by a fixed time method. The decrease in absorbance after 5 min was markedly correlated to the concentration. The relative standard deviations obtained were 1.30 and 1.87 for CPL and ESL, respectively, in pure forms. Correlation coefficients were 0.9997 and 0.9999 for CPL and ESL, respectively. The detection limits were determined as (S/N = 3) were 20 ng ml(-1) for CPL and 50 ng ml(-1) for ESL. The proposed procedure was successively applied for the determination of both drugs in pharmaceutical preparations and in biological fluids.     

Application of some chemometric methods in conventional and derivative spectrophotometric analysis of acetaminophen and ascorbic acid

The multivariate methods, principal component regression (PCR) and partial least squares (PLS) were tested as a calibration procedure for simultaneous ultraviolet spectrophotometric determination of acetaminophen (AC) and ascorbic acid (AA). Determination of these compounds is important because of their pharmacotherapeutic advantages. Due to spectral overlapping of AC and AA, PCR and PLS were used for construction of the calibration sets. The concentration linear range of AC and AA were 1.5–24.2 and 1.8–21.1 µg mL^?1 respectively. The absorption spectra were recorded from 215–310 nm. The minimum root mean square error of prediction (RMSEP) was 1.3507 and 0.4088 for AC and AA, by PLS, 0.7525 and 0.4015 by PCR in original data and 0.9454 and 0.2875, by PLS and 1.0386 and 0.4000 by PCR in derivative data. The procedure allows the simultaneous determination of AC and AA in synthetic mixtures and real sample solutions made up from pharmaceutical products, human serum and urine. Copyright © 2010 John Wiley & Sons, Ltd.     

Redox methods validation of paracetamol and ascorbic acid in pharmaceutical preparations

The contents of active substances were determined in a preparation TP-4 (tablets) containing paracetamol, ascorbic acid, caffeine and phenylephrine hydrochloride. For the determination of paracetamol and ascorbic acid a non-specific (cerometric and titration of 2,6-dichloroindophenol) method based on a redox reaction was used. Validation of the methods, performed on model mixtures, proved those methods to be accurate, precise, reproducible and linear within the range from 50% to 150% of the amount declared in the preparation. The content of paracetamol and ascorbic acid in TP-4, Thompayrin, Panadol Extra, Ring N, Polopiryna C, Efferalgan Vitamin C and Vitaminum C 0.2 satisfies the FP V demands (+/- 10% of the declared amount).     

Simultaneous determination of fosinopril and hydrochlorothiazide in pharmaceutical formulations by spectrophotometric methods

Three new spectrophotometric procedures for the simultaneous determination of fosinopril and hydrochlorothiazide are described. The first method, derivative-differential spectrophotometry, comprised of measurement of the difference absorptivities derivatized in the first-order (ΔD₁) of a tablet extract in 0.1 N NaOH relative to that of an equimolar solution in methanol at wavelengths of 227.6 and 276.4 nm, respectively. The second method, depends on the application ratio spectra derivative spectrophotometric method to resolve the interferance due to spectral overlapping. The analytical signals were measured at 237.9, 243.8 nm for fosinopril and 262.4, 269.3 and 278.6 nm for hydrochlorothiazide in the binary mixture, in the first derivative of the ratio spectra of the mixture solutions in methanol. Calibration graphs were established for 4.0–50.0 μg ml⁻¹ fosinopril and 2.0–14.0 μg ml⁻¹ hydrochlorothiazide in binary mixture. The third method, absorbance ratio method, the determination of fosinopril and hydrochlorothiazide was performed by using the absorbances read at 210.0, 219.5 and 271.7 nm in the zero-order spectra of their mixture. The developed methods were compared with absorbance ratio method. Application of the suggested procedures were successfully applied to the determination of this compound in synthetic mixtures and in pharmaceutical preparations, with high percentage of recovery, good accuracy and precision.     

Selective and validated spectrophotometric methods for the determination of nicorandil in pharmaceutical formulations

Two simple and sensitive validated spectrophotometric methods have been described for the assay of nicorandil in drug formulations. Method A is based on the reaction of the drug with phloroglucinol-sulfanilic acid reagent in sulfuric acid medium to give yellow-colored product, which absorbs maximally at 425 nm. Method B uses the oxidative coupling of 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) with DL- 3,4 - dihydroxyphenylalanine (DL-dopa) in the presence of nicorandil as oxidant in sulfuric acid medium to form an intensely colored product having maximum absorbance at 530 nm. Beer's law is obeyed in the concentration range 2.5 to 50.0 and 1.0 to 15.0 microg mL(-1) with methods A and B, respectively. Both methods have been successfully applied for the analysis of drug in pharmaceutical formulations. The reliability and the performance of the proposed methods are established by point and interval hypothesis and through recovery studies. The experimental true bias of all samples is smaller than +/-2%.     

Derivative spectrophotometric method for simultaneous determination of clindamycin phosphate and tretinoin in pharmaceutical dosage forms

A derivative spectrophotometric method was proposed for the simultaneous determination of clindamycin and tretinoin in pharmaceutical dosage forms. The measurement was achieved using the first and second derivative signals of clindamycin at (¹D) 251 nm and (²D) 239 nm and tretinoin at (¹D) 364 nm and (²D) 387 nm.The proposed method showed excellent linearity at both first and second derivative order in the range of 60–1200 and 1.25–25 μg/ml for clindamycin phosphate and tretinoin respectively. The within-day and between-day precision and accuracy was in acceptable range (CV<3.81%, error<3.20%). Good agreement between the found and added concentrations indicates successful application of the proposed method for simultaneous determination of clindamycin and tretinoin in synthetic mixtures and pharmaceutical dosage form.     

HPLC methods for choloroquine determination in biological samples and pharmaceutical products

ObjectiveReview and assess pharmaceutical and clinical characteristics of chloroquine including high-performance liquid chromatography (HPLC)-based methods used to quantify the drug in pharmaceutical products and biological samples.Evidence acquisitionA literature review was undertaken on the PubMed, Science Direct, and Scielo databases using the following keywords related to the investigated subject: ‘chloroquine’, ‘analytical methods’, and ‘HPLC’.ResultsFor more than seven decades, chloroquine has been used to treat malaria and some autoimmune diseases, such as lupus erythematosus and rheumatoid arthritis. There is growing interest in chloroquine as a therapeutic alternative in the treatment of HIV, Q fever, Whipple’s disease, fungal, Zika, Chikungunya infections, Sjogren’s syndrome, porphyria, chronic ulcerative stomatitis, polymorphic light eruption, and different types of cancer. HPLC coupled to UV detectors is the most employed method to quantify chloroquine in pharmaceutical products and biological samples. The main chromatographic conditions used to identify and quantify chloroquine from tablets and injections, degradation products, and metabolites are presented and discussed.ConclusionResearch findings reported in this article may facilitate the repositioning, quality control, and biological monitoring of chloroquine in modern pharmaceutical dosage forms and treatments.Graphical abstract      

Selective and validated kinetic spectrophotometric method for the determination of irbesartan in pure and pharmaceutical formulations

1. Download high-res image (93KB)
2. Download full-size image

     

Differential spectrophotometric determination of tyrosine and tryptophan in pharmaceutical amino acid solutions.

A method is proposed for the simultaneous determination of tyrosine and tryptophan in solutions by differential spectrophotometry. The concentrations are calculated from the measurement of the absorbance of the amino acid mixture in an alkaline medium and from the differential absorbance of the alkaline solution against the acid solution at 294.4 nm. A comparison with three other well-known methods is discussed.     

Comparison of spectrophotometric and colorimetric methods in determination of clavulanic acid

The spectrophotometric method for determination of clavulanic acid and amoxycillin after NaOH hydrolysis was elaborated.     

Automatic potentiometric flow titration procedure for ascorbic acid determination in pharmaceutical formulations

A flow procedure for the determination of ascorbic acid in pharmaceutical formulations exploiting potentiometric titration is described. The method is based on the reduction of IO₃⁻ by ascorbic acid and the detection was carried out employing a flow-through ion selective electrode for iodide. The flow network controlled by a microcomputer was designed to implement multicommutation for ease of operation and robustness. The titration system allowed the determination of ascorbic acid in pharmaceutical formulations with concentrations ranging from 7.5 to 15.0 mmol l⁻¹. No significant differences at the 95% confidence level were observed in comparison with results obtained by a manual procedure. Merit figures of results such as a relative standard deviation of 1.0% (n=6) and a reagent consumption of 21.4 mg IO₃⁻ per determination were obtained.     

Three new spectrophotometric methods applied to the simultaneous determination of hydrochlorothiazide and irbesartan

This work involves the simultaneous determination of hydrochlorothiazide and irbesartan in a binary mixture without previous separation by three new analytical methods. The first method, based on compensation technique, is presented for the derivative spectrophotometric determination of binary mixtures with overlapping spectra. By using ratios of the derivative maxima or the derivative minimum, the exact contribution of either component in the binary mixture can be measured and the amounts quantified. The second method uses of the first derivative of the ratio spectra. The ratio spectra were obtained by dividing the absorption spectra of the binary mixture by that of one of the components. The amplitudes in the first derivative of the ratio spectra at 231, 266, 279, 238 and 248 nm were selected to determine hydrochlorothiazide and irbesartan in binary mixtures. The concentration of the other components are then determined from their respective calibration graphs treated similarly. With the third method, the absorbance ratio method, the determination of hydrochlorothiazide and irbesartan was performed using the absorbances read at 272 nm, 241 nm and 263 nm in the zero-order spectra of their mixture. The absorbance ratio was also developed as a comparison method. The three methods are simple, accurate, rapid and require no preliminary separation steps and can, therefore, be used for routine analysis of both drugs in quality control laboratories.     

Simultaneous spectrophotometric determination of mefenamic acid and paracetamol in a pharmaceutical preparation using ratio spectra derivative spectrophotometry and chemometric methods

Four new methods are described for the simultaneous determination of mefenamic acid (MEF) and paracetamol (PAR) in their combination. In the first method, ratio spectra derivative method, analytical signals were measured at the wavelengths corresponding to either maximums or minimums for both drugs in the first derivative spectra of the ratio spectra obtained by dividing the standard spectrum of one of two drugs in 0.1 M NaOH:methanol (1:9). In the chemometric techniques, classical least-squares, inverse least-squares and principal component regression (PCR), the training was randomly prepared by using the different mixture compositions containing two drugs in 0.1 M NaOH:methanol (1:9). The absorbance data was obtained by the measurements at 13 points in the wavelength range 235–355 nm in the absorption spectra. Chemometric calibrations were constructed by the absorbance data and training set for the prediction of the amount of MEF and PAR in samples. In the third chemometric method, PCR, the covariance matrix corresponding to the absorbance data was calculated for the basis vectors and matrix containing the new coordinates. The obtained calibration was used to determine the title drugs in their mixture. Linearity range in all the methods was found to be 2–10 μg/ml of MEF and 4–20 μg/ml of PAR. Mean recoveries were found satisfactory (>99%). The procedures do not require any separation step. These methods were successfully applied to a pharmaceutical formulation, tablet, and the results were compared with each other.     

Optimization of the spectrophotometric method for quantitative determination of ascorbic acid in medicinal forms

A modified method for determination of ascorbic acid is developed. Its metrological characteristics are determined. Two procedures for quantitative determination of ascorbic acid in medicinal forms are compared. The modified method has advantages over the traditional titration method. The modified method can be applied to quantitative determination of ascorbic acid in injectable medicinal forms.     

Comparison of two derivative spectrophotometric methods for the determination of alpha-tocopherol in pharmaceutical preparations

Simple, sensitive and reliable derivative spectrophotometric methods were developed and validated for determination of alpha-tocopherol in pharmaceutical preparations. The solutions of standard and the sample were prepared in absolute ethanol. The quantitative determination of the drug was carried out using the first derivative values measured at 284, 304 nm and the second derivative values measured at 288, 296 nm. Calibration graphs constructed at their wavelengths of determination were linear in the concentration range of alpha-tocopherol using peak to zero 10-250 microg ml(-1) for first and second derivative spectrophotometric methods. Developed spectrophotometric methods in this study are accurate, sensitive, precise, reproducible, and can be directly and easily applied to Evon dragee form as pharmaceutical preparation. Statistical analysis (Student's t-test) of the obtained results showed no significant difference between the proposed two methods.     

Simultaneous spectrofluorimetric and spectrophotometric determination of melatonin and pyridoxine in pharmaceutical preparations by multivariate calibration methods

Partial least-squares (PLS) calibration and principal component regression (PCR) methods were utilized for the simultaneous spectrofluorimetric and spectrophotometric determination of pyridoxine (PY) and melatonin (MT). Since emission and adsorption spectra of these drugs overlap, PY and MT cannot be directly determined by fluorimetric nor by spectrophotometric methods. Full-spectrum multivariate calibration PLS and PCR methods were developed for both fluorimetry and spectrophotometry. The conditions were optimized for fluorimetric as well as for spectrophotometric determination of both drugs. The simultaneous determination of PY and MT was carried out in mixtures by recording the emission fluorescence spectrum between 324 and 500 nm (lambda(ex) 285 nm) for fluorimetry, and by recording the absorption spectrum between 250 and 350 nm for spectrophotometry (lambda(max(PY)) 310 nm, lambda(max(MT)) 278 nm). The experimental calibration matrixes were designed orthogonally. At the optimum conditions, dynamic ranges were 0.04-1.3 and 0.1-4 microg ml(-1) for fluorimetry and 1-22 and 1-24 microg ml(-1) for spectrophotometry for MT and PY, respectively. The calibration concentrations were prepared in the dynamic ranges. The parameters of the chemometrics procedure for the simultaneous determination of MT and PY were optimized, and the proposed methods were validated with prediction set. Finally the procedures were successfully applied to simultaneous spectrofluorimetric and spectrophotometric determination of PY and MT in synthetic mixtures and in a pharmaceutical formulation.