Derivative Spectrophotometric Method Research Articles

Quantitative determination of Dapoxetine Hydrochloride and Tadalafil using different validated spectrophotometric methods.

Three rapid, simple and selective spectrophotometric methods were developed for determination of Dapoxetine Hydrochloride (DAP) and Tadalafil (TAD) in bulk and pharmaceutical dosage forms. Method (A) is simultaneous first derivative (1D) spectrophotometric method in which the peak amplitudes of the first derivative spectra (1D) were measured for both DAP and TAD at 322.4 nm and 230 nm, respectively with no interference from each other. Method (B) is the area under curve (AUC) spectrophotometric method in which the areas under curve in the wavelength ranges 228-240 nm and 242-254 nm are used for determination of DAP and TAD respectively. Method (C) is ratio subtraction combined with extended ratio subtraction spectrophotometry (EXRS) in which TAD was determined by dividing the mixture spectra by the spectrum of 15 μg/mL solution of DAP, while DAP was be determined by dividing the mixture spectra by the spectrum of 30 μg/mL solution of TAD. The developed methods were applied to different laboratory prepared mixtures of DAP and TAD. These methods were validated according to the ICH guidelines with respect to linearity, accuracy, precision, selectivity and specificity, and can be used for routine quality control analysis of DAP and TAD in their dosage forms.

Development and Validation of First Order Derivative Spectrophotometric Method for Simultaneous Estimation of Rutin Trihydrate and Trigonelline Hydrochloride in Antidiabetic Herbal Formulation

Development and Validation of First Order Derivative Spectrophotometric Method for Simultaneous Estimation of Rutin Trihydrate and Trigonelline Hydrochloride in Antidiabetic Herbal Formulation

Mean centering-triple divisor and ratio derivative-zero crossing for simultaneous determination of some diabetes drugs in their quaternary mixture with severely overlapping spectra

Two ratio derivative spectrophotometric methods were performed for the simultaneous analysis of metformin hydrochloride, empagliflozine, linagliptin, and pioglitazone hydrochloride in their synthetic mixtures without prior chemical separation. The drugs are approved for the treatment of type 2 diabetes. Despite the various advances in the management of diabetes, it remains to be the major cause of disability and morbidity, including blindness, amputation, heart disease, peripheral neuropathy, and kidney disease. These techniques consisted of several steps using ratio and derivative spectra. The absorption spectra of the mentioned drugs were recorded in the range of 200-350 nm, which have the concentration ranges of 1.0-10, 2.5-30, 5.0-40, and 2.5-30 μg mL-1 for metformin hydrochloride, empagliflozine, linagliptin, and pioglitazone hydrochloride, respectively, using zero-order spectra. The mean centring of ratio spectra combined with triple divisor were measured at the amplitude values 242, 256, 272 and 296 nm for metformin hydrochloride, empagliflozine, linagliptin and pioglitazone hydrochloride, respectively; the derivative ratio spectra-zero crossing quantifies the amplitude value of the analytical signal at 234, 244, 260 and 280 nm for metformin hydrochloride, empagliflozine, linagliptin and pioglitazone hydrochloride, respectively. The method was validated according to the ICH guidelines, accuracy, precision and repeatability were found to be within the acceptable limits. Finally, statistical comparisons between the proposed methods and with the reported methods with respect to accuracy and precision show that no significant difference was found by using Student's t-test, the F-test and one-way ANOVA.

Development and validation of first and zero order derivative spectrophotometric methods for the determination of rilmenidine in pharmaceutical preparations and forced degradation study

Development and validation of first and zero order derivative spectrophotometric methods for the determination of rilmenidine in pharmaceutical preparations and forced degradation study

SECOND DERIVATIVE SPECTROPHOTOMETRIC METHOD FOR SIMULTANEOUS DETERMINATION OF DOXYLAMINE SUCCINATE AND PYRIDOXINE HCL IN PHARMACEUTICAL FORMULATIONS

Estimation of drugs in pharmaceutical formulations by using UV-Visible spectrophotometric method is one of the most frequently used techniques in pharmaceutical analysis. Simple and reliable second derivative spectrophotometric method was developed and validated for the simultaneous estimation of Doxylamine Succinate and Pyridoxine HCL in bulk and pharmaceutical formulations. The quantitative determination of the drugs was carried out using the second derivative values measured at 239 nm and 290 nm for Doxylamine Succinate and Pyridoxine Hcl respectively. The method has been developed and validated for the assay of Doxylamine Succinate and Pyridoxine HCL using methanol as diluents. Calibration graphs drawn at their wavelengths of determination were linear in the concentration range of 1-8 µg mL-1 for Doxylamine Succinate and 12.5 - 100 µg mL-1 for Pyridoxine Hcl. At 232 nm Doxylamine Succinate showed zero absorbance but Pyridoxine HCL had considerable amount of absorbance. Similarly at 290 nm Pyridoxine HCL showed zero absorbance but Doxylamine Succinate had considerable amount of absorbance. The limit of Quantification (LOQ) of Doxylamine Succinate and Pyridoxine HCL was found to be 0.6 µg mL-1 and 1µg mL-1 respectively and the limit of detection (LOD) was found to be 0.08 µg mL-1 and 0.3 µg mL-1 respectively. Comparison second derivative spectrum of Doxylamine Succinate and Pyridoxine HCL in standard and drug formulation solutions showed that the wavelength of maximum absorbance did not change. The low relative standard deviation values indicate good precision and high recovery values indicate accuracy of the proposed method. Developed second derivative spectrophotometric method was simple, accurate, precise, specific, sensitive and reproducible, which can be directly and easily applied to pharmaceutical dosage forms.

Simultaneous Determination of Moxifloxacin and Flavoxate by RP-HPLC and Ecofriendly Derivative Spectrophotometry Methods in Formulations.

Simple, fast, and precise reversed-phase (RP)-high-performance liquid chromatography (HPLC) and two ecofriendly spectrophotometric methods were established and validated for the simultaneous determination of moxifloxacin HCl (MOX) and flavoxate HCl (FLX) in formulations. Chromatographic methods involve the separation of two analytes using an Agilent Zorbax SB C18 HPLC column (150 mm × 4.6 mm; 5 µm) and a mobile phase consisting of phosphate buffer (50 mM; pH 5): methanol: acetonitrile in a proportion of 50:20:30 v/v, respectively. Valsartan was used as an internal standard. Analytes were monitored by measuring the absorbance of elute at 299 nm for MOX and 250 nm for FLX and valsartan. Two environmentally friendly spectrophotometric (first derivative and ratio first derivative) methods were also developed using water as a solvent. For the derivative spectrophotometric determination of MOX and FLX, a zero-crossing technique was adopted. The wavelengths selected for MOX and FLX were −304.0 nm and −331.8 nm for the first derivative spectrophotometric method and 358.4 nm and −334.1 nm for the ratio first-derivative spectrophotometric method, respectively. All methods were successfully validated, as per the International Conference on Harmonization(ICH) guidelines, and all parameters were well within acceptable ranges. The proposed analytical methods were successfully utilized for the simultaneous estimation of MOX and FLX in formulations.

Simultaneous ultrasonic-assisted removal of malachite green and methylene blue from aqueous solution by Zr-SBA-15

In this study, simultaneous and competitive removal of methylene blue (MB) and malachite green (MG) dyes was performed by employing nanostructure Zr-SBA-15, once using solid-phase extractionmethod (SPE) and again using ultrasonic bath, followed by second-order derivative spectrophotometric method in order to resolve the corresponding overlapped spectra. Zr-SBA-15 characterized by FT-IR, XRD, BET, SEM and EDX techniques. Using the proposed procedure, removal of the mentioned dyes was carried out in the minimum time. Moreover, some of the most influential parameters including the initial concentration of MB and MG, dosage of the absorbent, sonication time and pH of the medium were optimized using central composite design (CCD) in response surface methodology (RSM). Desirability scores demonstrated the optimal conditions as follows: sonication time of 4.78 min, adsorbent dosage of 6.66 mg, pH of 7.15 and initial concentrations of 10.21 and 5.48 mg L−1 for MB and MG, respectively. Under optimum conditions, maximum adsorption capacities of 310.88 and 140.61 mg g−1 were achieved for MB and MG, respectively. Kinetic studies and calculation of relevant equations from kinetic graphs and isotherm exhibited simultaneous adsorption of the desired dyes, followed by pseudo-second order spectrophotometric method and Langmuir isotherm.

Development of a Discriminative and Biorelevant Dissolution Test Method for Atorvastatin/Fenofibrate Combination with Appliance of Derivative Spectrophotometry.

Nowadays, the market is flooded with combinations of drugs in various dosage forms, but there is a lack of official methods to quantify them. A single dissolution test method for the analysis of combined dosage form is preferred for simplification of quality control testing. If the developed dissolution medium mimics the biorelevant and discriminating dissolution procedure for drug products with limited drug aqueous solubility it is a useful tool for qualitative forecasting of the in vivo behavior of formulations. Dissolution profiles were evaluated for atorvastatin and fenofibrate in capsules, using a paddle-type United States Pharmacopeia dissolution apparatus in 900 mL of medium at 50 rpm and 37±0.5°C. The best medium was 900 mL of 0.5% w/v sodium lauryl sulfate. The cumulative % dissolution was more than 85% within 45 min for marketed tablets. The proposed dissolution test conditions have discriminative power, dissimilarity factor (f1) values are low (12-16%), and similarity (f2) factor values are also low (45-48%). Hence the use of 0.5% w/v sodium lauryl sulfate solution is justified. The dissolution method was validated (% relative standard deviation <2). To quantify both drugs simultaneously, a second derivative spectrophotometric method was established (λmax 281 nm and 296 nm, respectively, for atorvastatin and fenofibrate) in acetate buffer, pH 2.8 solution.

On the determination of manganese in the presence of iron in pregnant leach solution using derivative spectrophotometry

Mn determination in samples with high Fe content using derivative spectrophotometric method was proposed in this paper, which formaldoxime was used as chromogenic reagent. The derivative method is useful to manipulate spectra data in order to eliminate the noise spectra i.e. Fe and isolate the spectra of elements of interest (Mn). Formaldoxime was chosen since the reagent reacted both to Mn and Fe at the same pH condition. In this paper, the accuracy in Mn determination in the presence of Fe using proposed method would be assessed and discussed. Mn and Fe could be simultaneously determined Mn using zero crossing point of first derivative Fe-formaldoximate spectra at 530 nm for Mn determination, while Fe could be predicted using zero crossing point of second derivative Mn-formaldoximate spectra at 469 nm. Maximum concentration which obeyed the linearity of calibration curve is 2 and 20 mg/L for Mn and Fe, respectively. The error in Mn and Fe prediction depends on ratio of both elements.

NOVEL ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF BROMOFENAC SODIUM IN BULK AND PHARMACEUTICAL DOSAGE FORM BY DERIVATIVE AND AUC SPECTROSCOPIC METHOD

The present study was carried out to develop a simple and reliable derivative spectrophotometric method for the determination of bromofenac sodium in pharmaceutical dosage forms .The solutions of standard and the sample were prepared in distilled water The quantitative determination of the drug was carried out with zero order derivative (method A) values measured at 268 nm and first order (method B) derivative values measured at 258 nm , and two wavelengths 262nm and 274nm were selected for the determination AUC (method C) of integrated areas. Calibration graphs constructed at their wavelengths of determination, were linear within the concentration range of 2-12 μg/mL (r2 = 0.999) for zero order and (r2 = 0.997) first order derivative spectrophotometric method. No significant difference between the performance of the proposed methods regarding the mean values and standard deviations and is suitable for the routine quality control application of bromofenac sodium in its pharmaceutical formulations.

Derivative UV Spectrophotometric Method for Validation of Imatinib mesylate in Bulk and Pharmaceutical Dosage Form

Simple and precise derivative UV spectrophotometric method by first and second order have been developed and validated for the estimation of imatinib mesylate in bulk and its tablet formulation. The standard and sample solutions of imatinib mesylate were prepared in distilled water. Imatinib mesylate was estimated by first and second order at wavelength 227nm and 205.5nm respectively. Beer's law was obeyed in the concentration range of 1 to 20μg/ml with coefficient of correlation value 0.9999. These methods were tested and validated for various parameters according to ICH guidelines. The precision expressed as relative standard deviation were 0.2429% for first order and 0.6873% for second order derivative method respectively. The proposed method was successfully applied for the determination of imatinib mesylate in pharmaceutical formulation. Results of the analysis were validated statistically and were found to be satisfactory. The proposed method is simple, easy to apply, low-cost and require relatively inexpensive instruments.

Determination of Food Colorants (Ponceau 4R and Brilliant black) by Derivative Spectrophotometry

Spectrophotometric method was developed and applied for simultaneous determination of two colorants: Ponceau 4R and Brilliant black in Syrian foodstuffs. This study was applied on several Syrian foodstuffs as: Royal Jelly, Archi jelly, Columbus drink (strawberry), Columbus drink (blueberry), Aquaz drink (blueberry). Derivative spectrophotometric method (DS) was applied for the determination of Ponceau 4R and Brilliant black, respectively. Ponceau 4R was determined by first derivative spectrophotometry (1D454), and Brilliant black was determined by first derivative spectrophotometry (1D624). Linearity ranges were 3–40 μg/mL for Ponceau 4R and 2–35 μg/mL for Brilliant black. Regression analysis showed a good correlation coefficients R2 = 1 and R2 = 0.9999 for Ponceau 4R and Brilliant black, respectively. The limit of detection (LOD) and limit of quantification (LOQ) were to be 0.825 μg/mL and 2.50 μg/mL for Ponceau 4R and 0.328 μg/mL and 0.99 μg/mL for Brilliant black, respectively. The proposed derivative method was successfully applied to analysis individual or mixture of Ponceau 4R and Brilliant black in foodstuffs. All studied samples showed dye levels conformity with Syrian legislation.

New first derivative spectrophotometric methods for the estimation of Bumetanide in tablet dosage forms

First derivative spectrophotometric methods have been developed for the assay of Bumetanide using Shimadzu UV-1800 Model double beam UV-VIS spectrophotometer in reagents such as hydrochloric acid, phosphate buffer pH 3.6, phosphate buffer pH 2.0 and distilled water. Bumetanide has shown linearity 10-70 µg/ml in all the methods and the linear regression equations are found to be y = 0.0015x - 0.0013 (R² = 0.9993), y= 0.0007x - 0.0004 (R² = 0.9991), y = 0.0014x - 0.0015 (R² = 0.9993) and y = 0.0014x - 0.0015 (R² = 0.9995) in hydrochloric acid, phosphate buffer pH 3.6, phosphate buffer pH 2.0, and distilled water respectively. The methods are validated as per ICH guidelines and found to be precise, simple and accurate.

Derivative Spectrophotometric method for Estimation of Secnidazole in Bulk and Pharmaceutical Dosage form

The objective of the study was to develop simple, accurate, precise and rapid UV first order derivative spectrophotometric methods with subsequent validation by using ICH guidelines for the determination of secnidazole in pharmaceutical dosage form. The proposed first order derivative methods involve the measurement of absorbance of drug at 305 nm for the estimation of secnidazole respectively. The linearity of the proposed methods were found in the concentration range of 2.5–15 μg/ml (r2= 0.9999) for method and the percentage mean recovery was found to be 100.01% respectively. The method was also statistically validated for its linearity, accuracy and precision. Both intra and inter day variation showed less percentage (%) RSD values indicating high grade of precision of these methods.

Derivative spectrophotometric methods for the assay of Glibenclamide (An anti-diabetic agent)

Glibenclamide is an anti-diabetic agent used for the treatment of diabetes mellitus type 2. First derivative spectrophotometric techniques were developed for the assay of Glibenclamide tablet dosage forms in three different reagents and the methods were validated. Glibenclamide has shown linearity over the concentration range 1-80, 1-100 and 1-80 µg/ml respectively in phosphate buffer pH 2.0 (Method A), phosphate buffer pH 8.0 (Method B) and borate buffer pH 9.0 (Method C) respectively. The methods were validated by precision and accuracy studies and are suitable for the determining the assay of Glibenclamide tablets.

Area under Curve and First Order Derivative Spectrophotometric Method and Development and Validation of Adenosine in Bulk drug

Area under Curve and First Order Derivative Spectrophotometric Method and Development and Validation of Adenosine in Bulk drug

Validated Derivative Spectrophotometric method for simultaneous estimation of Levocetirizine Dihydrochloride and Phenylephrine Hydrochloride from tablet formulations

Validated Derivative Spectrophotometric method for simultaneous estimation of Levocetirizine Dihydrochloride and Phenylephrine Hydrochloride from tablet formulations

Simultaneous removal of binary dye from textile effluent using cobalt ferrite-alginate nanocomposite: Performance and mechanism

The rapid removal of dye effluent containing two or more dyes is in demand due to its significant environmental issues. The present communication deals with the simultaneous adsorption of Reactive red 195 (RR195) and Reactive yellow 145 (RY145) from a textile dye effluent in a binary component system. Cobalt ferrite-alginate nanocomposite synthesized by ex-situ polymerization was employed as an adsorbent for the removal of binary dye effluent. The first order derivative spectrophotometric method was applied for the simultaneous quantification of RR195 and RY145 in binary solutions. The binary adsorption equilibrium could be achieved within 60 min, and the adsorption process followed pseudo second order kinetics. The removal efficiency could be maintained in a wide pH range of 3–6. The presence of amine, hydroxyl, carbonate and ferrite groups on the adsorbent surface played a vital role in the removal of RR195 and RY145 from their binary mixture. The continuous adsorption experiments revealed that the breakthrough time and exhaustion time increases with an increase in the bed height. The experimental results present new sustainable, cost effective biocompatible nanocomposite as a potential adsorbent for the removal of real-time dye effluent. Moreover, it is magnetically separable and reusable. The cobalt ferrite-alginate as a sole nanocomposite is capable of eliminating the whole dye content from a mixture and serves as a better solution for effective water remediation.

Development and Validation of Spectrophotometric Methods for the Determination of Amoxicillin trihydrate and Dicloxacillin sodium in Their Binary Mixture

Three sensitive and cost-effective spectrophotometric methods are introduced for the determination of amoxicillin and dicloxacillin in their binary mixtures with minimum sample pretreatment, with or without the presence of their common impurity; 6-aminopenicillanic acid (6-APA). In this work, dicloxacillin is determined by dual wavelength, derivative ratio and isoabsorptive spectrophotometric methods. However, amoxicillin is determined by direct UV spectrophotometry at 273.6 nm and by the first derivative ratio spectrophotometric method (DD method). For method (A); the dual wavelength method, the wavelengths selected for the determination of dicloxacillin were 223.6 and 237 nm. Method (B); the isoabsorptive spectrophotometric method, comprises measuring the total content of the mixture at their isoabsorptive point (230.4 nm), and then the content of dicloxacillin can be calculated by subtraction. Method (C) is the first derivative of ratio spectra for the determination of amoxicillin (using 8 μg/mL of dicloxacillin as a divisor at 231 nm) and dicloxacillin (using 20 μg/mL of 6-APA as a divisor at 234.6 nm) in presence of their common impurity; 6-APA. Statistical comparison of the results obtained from the suggested methods with those of the reported HPLC method showed no significant difference with respect to accuracy and precision. The developed methods can be used for quality control analysis of the studied drugs in laboratories lacking HPLC qualifications.Kay words: Amoxicillin, Dicloxacillin, Dual wavelength, Isoabsorptive point, First derivative ratio

Second Derivative Spectrophotometric Determination of Iron(II) and Ruthenium(III) Using 1, 10-phenanthroline

A simple and sensitive derivative spectrophotometric method has been developed for the determination of Fe(II) and Ru(III) using the baseline to peak measurement techniques. In the present method 1,10-phenanthroline (o-phen) used as a complexing agent. Fe(II) and Ru(III) forms a complex with o-phen at pH 5 and 4, respectively. Based on baseline-to-peak measurement techniques deep red Fe(II)-o-phen complex shows the maximum peak at 535 nm, while the yellow product of Ru(II) - o-phen complex at 466 nm. Beer's law obeyed in the range of 0.1 - 2.0 μg mL-1 for Fe(II) and 5.0 - 20.0 μg mL-1 for Ru(III) which is supported by correlation coefficient 0.99853 and 0.99914, respectively. The present method has been applied successfully for the determination of Fe (II) in pharmaceutical formulations and Ru(III) in some synthetic mixtures.