Simultaneous Determination Of Binary Mixtures Research Articles

Simultaneous Determination of Binary Mixture of Estradiol and Progesterone Using Different Spectrophotometric Methods

Four rapid, accurate and very simple derivative spectrophotometric techniques were developed for the quantitative determination of binary mixtures of estradiol (E2) and progesterone (PRG) formulated as a capsule. Method I is the first derivative zero-crossing technique, derivative amplitudes were detected at the zero-crossing wavelength of 239.27 and 292.51 nm for the quantification of estradiol and 249.19 nm for Progesterone. Method II is ratio subtraction, progesterone was determined at λmax 240 nm after subtraction of interference exerted by estradiol. Method III is modified amplitude subtraction, which was established using derivative spectroscopy and mathematical manipulations. Method IIII is the absorbance ratio technique, absorbance of both medicines was measured at two wavelengths λ1= 260, -absorptive point and λ2=240max of progesterone. The Q equations were used to calculate the final concentrations. The calibration curve is linear from 5.0–140 and 2.0–32.0 µg/ml for estradiol and progesterone respectively. The proposed techniques' selectivity was tested using synthetic combinations created in the lab and assessed using the standard addition method. Using one-way ANOVA, the outputs of the proposed ways were compared, and the result showed no significant differences between the proposed techniques.

Advanced Sensing Performance towards Simultaneous Determination of Binary Mixture of Antihypertensives Using PANI–Cerium Oxide Nanoparticles as Modifier in Carbon Paste Incorporating Graphite and Silicon-Oil

Present paper reports multianalyte electroanalysis of hypertensive having amlodipine and nebivolol molecules in a single dose. Amlodipine and Nebivolol exhibited oxidation peaks at 0.70 and 0.90 V respectively on the Graphite/Polyaniline-Cerium Oxide/Carbon paste electrode. The linearity range was 0.1 to 1.6 μg ml−1 in Britton Robinson buffer (pH 8.0). The limit of detection was 20.0 ng ml−1 for Amlodipine and 30.0 ng ml−1 for Nebivolol and the limit of quantification was 80.0 ng ml−1 for Amlodipine and 100 ng ml−1 for Nebivolol respectively. These analytes were also determined in pharmaceutical formulation and human serum and good recovery was obtained for the developed method.

Two different spectrophotometric methods for simultaneous determination of binary mixture of atenolol and amlodipine in commercial formulation

Two different spectrophotometric methods for simultaneous determination of binary mixture of atenolol and amlodipine in commercial formulation

Simultaneous Determination of Binary Mixtures of Aniline and 2-Nitronailine in Tap Water Samples by Derivative Spectrophotometry

Simultaneous Determination of Binary Mixtures of Aniline and 2-Nitronailine in Tap Water Samples by Derivative Spectrophotometry

Spectral manipulation of ratio data for simultaneous determination of binary mixture of Paracetamol and Phenylephrine Hydrochloride

Three ratio spectra manipulating spectrophotometric methods have been developed for determination of Paracetamol (PAR) and Phenylephrine HCl (PHE) in bulk powder and in pharmaceutical formulation. Linear correlations were obtained over the concentration range of 1.0–25.0 µg/mL and 5.0–50.0 µg/mL for PAR and PHE, respectively. The first method is the ratio subtraction method (RS) coupled with constant multiplication (CM) in which PHE was determined by ratio subtraction and PAR was determined by constant multiplication. The second method is the ratio difference method (RD) which depends on measuring the difference between the amplitudes of the ratio spectra at two selected wavelengths. The third method is the first derivative of the ratio spectra (1DD), which allows the determination of PAR at 238.8 and 243 nm and PHE at 213.2, 222.2, 271.8 and 286 nm. The proposed methods are simple, accurate and precise (RSD does not exceed 2%). The applicability of the proposed methods was successfully verified by the analysis of PAR and PHE in pharmaceutical formulation without interference of the dosage form additives. Furthermore, the developed methods were validated according to ICH guidelines, so they are considered to be potential competitors for the analysis of the mixture in quality control labs and pharmaceutical factories.

Development of hybrid spectrofluorimetric method for simultaneous determination of Valsartan and Sacubitril in LCZ696 tablets

A hybrid Spectrofluorimetric method was developed for the simultaneous determination of binary mixtures, without prior separation steps. It coupled synchronous spectrofluorimetry with derivative ratio mathematical treatment. The method was applied successfully to quantify a new model binary mixture consisting of Valsartan (VAL) and Sacubitril (SAC). This mixture was recently approved by FDA as LCZ696. It added a great value in reducing morbidity and mortality in resistant heart failure (HF) patients. First derivative ratio synchronous fluorescence was measured at 258–295 (peak-to-peak) and 204 nm for VAL and SAC, respectively. ICH guidelines were fulfilled for the method validation. VAL and SAC showed linear responses in the range of 60–200 and 20–200 ng mL−1, respectively. The proposed method was compared, in details, with the reported ones. Its high accuracy, selectivity, simplicity and affordable cost recommend method application in large-scale routine analysis of LCZ696 tablets. Moreover, reliable application of this new integrated spectrofluorimetric method suggests expansion of its application for various therapeutic combinations and different matrices.

Determination of benazepril HCl and hydrochlorothiazide in pharmaceutical preparations using UV-visible spectrophotometry and genetic multivariate calibration method

Simultaneous determination of binary mixtures of benazepril and hydrochlorothiazide in pharmaceutical tablets using UV-visible spectrophotometry, classical least squares (CLS) and three genetic algorithms (GA) based multivariate calibration methods was demonstrated. The three genetic multivariate calibration methods are Genetic Classical Least Squares (GCLS), Genetic Inverse Least Squares (GILS) and Genetic Regression (GR). The sample data set contains the UV- spectra of 28 synthetic mixtures of benazepril (12∼36 μg/mL) and hydrochlorothiazide (10∼22 μg/mL) and 16 tablets containing both compounds. The spectra cover the range from 210 to 360 nm in 0.1 mn intervals. Several calibration models were built with the four methods. The root mean square error of calibration (RMSEC) and validation (RMSEV) for the synthetic data were in the range of 0.19 and 0.34 μg/mL for all the genetic algorithm based methods. The root mean square error of Prediction (RMSEP) values for the tablets were in the range of 0.04∼0.20 mg/tablets. A comparison of genetic algorithm selected wavelengths for each component was also included.

Development and Validation of Novel Spectro- Chemometric, Chemometric and TLC-Densitometric Methods for Simultaneous Determination of Timolol and Travoprost in their Bulk Powders and Pharmaceutical Formulation

Simple, sensitive and reliable spectro-chemometric, Chemometric and thin layer chromatography (TLC)-densitometric methods were developed for simultaneous determination of binary mixture of timolol (TIM) and travoprost (TRA) without prior separation in their bulk drugs and dosage forms. The speectro-chemometric methods used are derivative spectrophotometry and isosbestic point methods.

Development and validation of Novel Spectro-chemometric and high performance liquid chromatography methods for simultaneous determination of binary mixture of etilefrine hydrochloride and chlorpheniramine maleate in their bulk powders and different pharmaceutical formulations

Simple, sensitive and reliable spectro-chemometric and high performance liquid chromatography (HPLC) methods were developed for simultaneous determination of binary mixture of etilefrine hydrochloride and chlorpheniramine maleate without prior separation in their bulk drugs and dosage forms. The spectro-chemometric methods used are, derivative spectrophotometry, derivative ratio, and isosbestic point methods. The HPLC method involves the use of reversed-phase separation mode using eluant of pH 3.5, consisted of phosphate buffer/acetonitrile (30:70 v/v) and Zorbax ODS column. All variables influencing the spectrophotometric and HPLC methods were carefully investigated and optimized. The developed methods were evaluated according to United State Pharmacopeia (USP) and International Conference of Harmonization (ICH) rules. The current methods were successfully implemented for direct the determination of these drugs in their trade pharmaceutical formulations. The obtained results were contrasted with those calculated after application of reference method. The data obtained from both methods were statistically analyzed by F- and t-tests. The results of such study showed excellent agreement in respect to the accuracy and precision of the suggested and reference methods.

Application of derivative emission fluorescence spectroscopy for determination of ibuprofen and phenylephrine simultaneously in tablets and biological fluids.

Two sensitive, rapid, and accurate derivative emission spectrofluorimetric methods applying zero crossing techniques were developed for simultaneous determination of binary mixtures of ibuprofen (IBU) and phenylephrine hydrochloride (PHE) in pure powder, synthetic mixture and combined tablets. The proposed methods were performed via measuring the intersected drug derivative amplitude of one drug at the zero crossing points for the other one and vice versa. The two methods rely on the measurement of the combined drugs native fluorescence after excitation at 270 nm in methanol directly, followed by differentiation using first (D1) and second derivative (D2) techniques. Applying the D1, IBU was measured quantitatively at 293.1 nm at zero crossing of PHE, on the other side; PHE was measured quantitatively at 300.7 nm at zero crossing of IBU. By the same way, applying the D2, the wavelengths selected were 303.5 nm for IBU and 312.9 nm for PHE. The concentration plots of derivative fluorescence intensity were rectilinear over the range of 0.5-10 μg/mL and 0.025-0.5 μg/mL for IBU and PHE, respectively. The results obtained with average % recoveries ± RSD are 99.73 ± 0.72 (IBU, D1), 99.49 ± 0.95 (PHE, D1), 99.79 ± 0.47 (IBU, D2), and 99.88 ± 0.34 (PHE, D2) were in good agreement with the comparison method. The proposed methods offer high sensitivity that enable direct analysis of IBU and PHE in spiked human plasma. The proposed methods were entirely validated in terms of ICH guidelines.

A Comparative Study of Smart Spectrophotometric Methods and a Densitometric Method for Simultaneous Determination of Binary Mixture of Canagliflozin and Metformin Hydrochloride

Simple and sensitive Spectrophotometric methods and a densitometric thin layer chromatographic method (TLC) are developed and validated for simultaneous determination of binary mixture of metformin hydrochloride (MET) and canagliflozin (CFZ) in combined dosage form. Three spectrophotometric methods manipulating ratio spectra namely ratio subtraction, ratio difference and derivative ratio are used for the determination of MET in the presence of CFZ without preliminary separation, while CFZ is directly determined by measuring its absorbance at λmax 290 nm. The calibration curves follow Beer's law in the concentration range of 1 - 20 and 1 - 30 μg/mL for MET and CFZ respectively. A simple TLC method is developed where separation is performed on TLC silica gel plates 60F254 using toluene: Methylene chloride: methanol: water: glacial acetic acid in the volume ratio (20:15:15:1:0.25) as a mobile phase. Rf values are 0.55 ± 0.05 for CFZ and 0.21 ± 0.03 for MET, the linearity ranges are 0.3-4.5 and 0.5-5.5 μg/band for CFZ and MET respectively. The developed methods are successfully applied for the simultaneous determination of MET and CFZ in bulk and pharmaceutical formulation.

Chromatographic methods for the simultaneous determination of binary mixture of Saxagliptin HCl and Metformin HCl

Two chromatographic methods were suggested for the simultaneous determination of a binary mixture containing Saxagliptin HCl (SAG) and Metformin HCl (MET). First method was RP-HPLC method. Chromatographic separation was done on Kinetex™ column–C18 (4.6×150mm, 2.6µm) using mobile phase consisted of acetonitrile:phosphate buffer pH=4.5 ±0.1 adjusted with orthophosphoric acid (13:87, v/v). Isocratic elution at a flow rate 1.5mL/min and UV detection at 220.0nm was performed. Second method was spectro-densitometric method. Chromatographic separation was done on precoated silica gel aluminium plates 60 F254 as a stationary phase and developing system consisting of chloroform:methanol:formic acid (80:20:0.3, by volume). The density of the separated bands was measured by UV detector at 210.0nm. The proposed methods were validated as per the ICH guidelines parameters like Linearity, precision, accuracy, selectivity, limit of detection and limit of quantitation. Statistical comparison was done between the obtained results and those obtained by the reported methods, showing no significant difference with respect to accuracy and precision.

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Spectrophotometric techniques were developed for the determination of single and binarymixture Promethazine hydrochloride (PMH) and Paracetamol (PCM). Normal and first derivative ( 1 D) used for single drug at λ 249.5 and 243.0 for PMH and 243.5 and 225 for PCM. The simultaneous determination of binary mixture (PMH) and (PCM) were accomplished by first derivative ( 1 D) and second derivative ( 2 D) spectrophotometric technique with applying zerocrossingat valley (V=216.5) and Peak (P=258.8)nm for (PMH) and (V=274.0 and P=299.2 nm for PCM).The correlation coefficient for calibration curves not less than 0.999 and the relative standard deviation not exceed to 0.214. The recovery of individual constituents under establishedconditions inthe ranges from 97.00% to 101.97 %. Linearity is maintained within a wide concentrationrange from 4.00-30.00mg/L for PMH and PCM. Standard addition method used forpharmaceutical tablets. A good accuracy and precision of simultaneous determination of (PCM), and (PMH) were confirmed by statistical analysis. The proposed procedures were successfully applied to the determination of these compounds in different ratio by synthetic mixtures and pharmaceutical tablets without requiring any separation step.

Ionic Liquid Crystals Modifier for Selective Determination of Terazosin Antihypertensive Drug in Presence of Common Interference Compounds

Electrochemical sensor was fabricated based on carbon paste electrode modified with an ionic liquid crystal ILC (2-chloro-1,3-dimethyl-imidazolidinium hexafluorophosphate) in presence of sodium dodecyl sulfate for the selective electrochemical determination of Terazosin (TZ) in presence of common interference compounds. The electrode performance was compared in presence of other ionic liquids ILs (1-Butyl-4-methyl pyridinium tetrafluoroborate) and (1-n-Hexyl-3-methyl imidazolium tetrafluoroborate). Ultrasensitive determination of Terazosin HCl at the ILC modified electrode in the linear dynamic ranges of 0.002 to 0.09 μmol·L−1 and 0.2 to 30 μmol·L−1 with correlation coefficients 0.996 and 0.995 and LODs 1.69 × 10−11 mol·L−1 and 6.43 × 10−9 mol·L−1, respectively, were obtained. Selective determination of TZ in presence of uric acid and ascorbic acid and simultaneous determination of binary mixtures of TZ/dopamine, TZ/paracetamol and TZ/Morphine were also determined successfully using the modified sensor.

Effective and Facile Determination of Vitamin B6 in Human Serum with CuO Nanoparticles/Ionic Liquid Crystal Carbon Based Sensor

New insights in fabrication of a sensitive, carbon nanotubes-based electrochemical sensor for determination of vitamin B6 (PY) are presented in this work. This was achieved by exploring the interesting properties of a conductive composite based on manual casting of successive layers of carbon nanotubes mixed with ionic liquid crystal and CuO nanoparticles (GC/(ILC-CNTs)/CuO) over glassy electrode surface. The proposed sensor was successfully used for the simultaneous determination of binary mixtures of PY and other vitamins (B2, B9, B12 or C) with good resolution. Under optimized conditions, a linear calibration curve was obtained for the determination of vitamin B6 in blood serum within the range 0.5 μmol L−1 to 50 μmol L−1 with sensitivity of 877 μA/mmol L−1, detection limit of 3.09 nmol L−1 and limit of quantification 10.31 nmol L−1. Furthermore, the recovery results of real blood serum samples proved excellent using the proposed composite which makes it a potential candidate for PY routine analysis.

Determination of binary mixture of ibuprofen and famotidine by different spectrophotometric methods

Four simple and specific spectrophotometric methods were developed and validated for the simultaneous determination of binary mixture of ibuprofen and famotidine, using unified regression equation. The proposed spectrophotometric procedures including, derivative ratio, ratio subtraction, dual wavelength and mean centering of ratio spectra do not require any separation steps. Accuracy, precision and linearity ranges of the proposed methods were determined and the specificity was assessed by analysing synthetic mixtures of both drugs. The methods were applied to a pharmaceutical formulation and the results obtained showed that there is no significant difference between the proposed methods and the reported one regarding both accuracy and precision.

Comparative study on four spectrophotometric methods manipulating ratio spectra for the simultaneous determination of binary mixture of diflucortolone valerate and isoconazole nitrate

Four simple, accurate, reproducible and non-sophisticated spectrophotometric methods manipulating ratio spectra were developed and validated for the simultaneous determination of diflucortolone valerate (DIF) and isoconazole nitrate (ISO) without preliminary separation in pure powder form and in their cream formulation. Method A, is constant center spectrophotometric method (CC), method B is a ratio difference spectrophotometric one (RD), method C is the first derivative of the ratio spectra (1DD), while method D is the mean centering of ratio spectra (MC). Linearity correlations ranges were 5–60μgmL−1 for DIF and 65–850μgmL−1 for ISO. The mean percentage recoveries of DIF were 101.60±1.056 for method A, 101.33±0.702 for method B, 101.31±1.476 for method C and 102.69±1.009 for method D, respectively. For ISO were 100.59±0.525 for method A, 99.68±0.721 for method B, 99.67±0.742 for method C and 101.37±0.958 for method D, respectively. Assessment of the specificity was achieved by analyzing synthetic mixtures containing the cited drugs. The four methods were applied for the determination of the cited drugs in cream formulation and the statistical comparison of the obtained results was made with each other and with those of official methods. The comparison in pure powder form showed that there is no significant difference between the proposed methods and the official methods regarding both accuracy and precision.

HPLC and TLC chromatographic methods for simultaneous determination of binary mixture of isoconazole nitrate and diflucortolone valerate

HPLC and TLC-densitometric methods were used to determine a binary mixture of isoconazole (ISO) and diflucortolone (DIF). For HPLC method a rapid separation could be achieved on a C18 column using mobile phase of 80% acetonitrile–20% methanol. The components were monitored at 230nm over a concentration range of 10–90μgmL−1 for ISO and 2–18μgmL−1 for DIF with mean percentage recoveries 99.95±0.866 and 99.98±0.744, respectively. The second method is TLC-densitometric, where ISO and DIF are separated on silica gel plates using ethyl acetate: chloroform: toluene (60:10:10 by volume) as a developing system and scanning of the separated bands at 215nm over a concentration range of 0.1–4μgspot−1 for ISO and scanning of the separated bands at 237nm over a concentration range of 0.1–1.4μgspot−1 for DIF with mean percentage recoveries 100.19±0.956 and 100.1±0.689 for ISO and DIF, respectively. The suggested methods were used to determine both drugs binary mixture in pure form and dosage form. The validity of the proposed methods was further assessed by applying standard addition technique. The obtained results were statistically compared with official HPLC method, showing no significant difference with respect to accuracy and precision.

Chemometrics-Enhanced Micelle-Mediated Extraction Spectrophotometric Method for Simultaneous Determination of Cu2+ and Zn2+ in Medicinal Plant, Rice and Water Samples Using Continuous Wavelet Transform

A new micelle-mediated extraction method for the pre-concentration of trace amounts of Cu2+ and Zn2+ as a prior step to their simultaneous spectrophotometric determination has been developed in various samples. The analytes were complexed with new synthesized ligand 4,4′-((4-chlorophenyl)methylene)bis(1,3-diphenyl-1H-pyrazol-5-ol) (CPBMPY) and Triton X-100 was added as a extraction agent. The optimal reaction and extraction conditions were optimized and the analytical characteristics of the method were obtained. The detection limit of the method was 0.90 and 0.30 ng mL−1 for Cu2+ and Zn2+, respectively. Continuous wavelet transformation (CWT) of visible spectra as a very simple and accurate method was developed for the simultaneous determination of binary mixtures of Cu2+ and Zn2+ ions. A zero-crossing technique was applied on the transformed signals and the constructed calibrations were tested by analyzing the composition of the different binary mixtures. The proposed procedure successfully was applied to analysis of water, rice, and medicinal plant and reference material samples. The amounts of metal ions obtained by the proposed methods were in good agreement with those obtained by Graphite furnace atomic absorption spectrometry.

Simultaneous determination of binary mixture of amlodipine besylate and atenolol based on dual wavelengths

Four, accurate, precise, and sensitive spectrophotometric methods are developed for simultaneous determination of a binary mixture of amlodipine besylate (AM) and atenolol (AT). AM is determined at its λmax 360nm (0D), while atenolol can be determined by four different methods. Method (A) is absorption factor (AF). Method (B) is the new ratio difference method (RD) which measures the difference in amplitudes between 210 and 226nm. Method (C) is novel constant center spectrophotometric method (CC). Method (D) is mean centering of the ratio spectra (MCR) at 284nm. The methods are tested by analyzing synthetic mixtures of the cited drugs and they are applied to their commercial pharmaceutical preparation. The validity of results is assessed by applying standard addition technique. The results obtained are found to agree statistically with those obtained by official methods, showing no significant difference with respect to accuracy and precision.