Development and Validation of Chemometric-Assisted Spectrophotometric Methods for Simultaneous Determination of Phenylephrine Hydrochloride and Ketorolac Tromethamine in Binary Combinations

2016 ◽  
Vol 99 (5) ◽  
pp. 1247-1251 ◽  
Author(s):  
Hamed M Elfatatry ◽  
Mokhtar M Mabrouk ◽  
Sherin F Hammad ◽  
Fotouh R Mansour ◽  
Amira H Kamal ◽  
...  
Keyword(s):  
Least Squares ◽  
Simultaneous Determination ◽  
Principal Component Regression ◽  
Principal Component ◽  
Data Matrix ◽  
Ketorolac Tromethamine ◽  
Concentration Data ◽  
Phenylephrine Hydrochloride ◽  
Spectrophotometric Methods

Abstract The present work describes new spectrophotometric methods for the simultaneous determination of phenylephrine hydrochloride and ketorolac tromethamine in their synthetic mixtures. The applied chemometric techniques are multivariate methods including classical least squares, principal component regression, and partial least squares. In these techniques, the concentration data matrix was prepared by using the synthetic mixtures containing these drugs dissolved in distilled water. The absorbance data matrix corresponding to the concentration data was obtained by measuring the absorbances at 16 wavelengths in the range 244–274 nm at 2 nm intervals in the zero-order spectra. The spectrophotometric procedures do not require any separation steps. The accuracy, precision, and linearity ranges of the methods have been determined, and analyzing synthetic mixtures containing the studied drugs has validated them. The developed methods were successfully applied to the synthetic mixtures and the results were compared to those obtained by a reported HPLC method.

scholarly journals Liquid Chromatographic and Spectrophotometric Determination of Diflucortolone Valerate and Isoconazole Nitrate in Creams

2011 ◽  
Vol 94 (1) ◽  
pp. 128-135 ◽  
Author(s):  
Elif Karacan ◽  
Mehmet Gokhan Çaġlayan ◽  
İsmail Murat Palabiyik ◽  
Feyyaz Onur
Keyword(s):  
Principal Component Regression ◽  
Principal Component ◽  
Derivative Spectrophotometry ◽  
Data Matrix ◽  
Concentration Data ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
First Derivative Spectrophotometry ◽  
Liquid Chromatographic

Abstract A new RP-LC method and two new spectrophotometric methods, principal component regression (PCR) and first derivative spectrophotometry, are proposed for simultaneous determination of diflucortolone valerate (DIF) and isoconazole nitrate (ISO) in cream formulations. An isocratic system consisting of an ACE® C18 column and a mobile phase composed of methanol–water (95+5, v/v) was used for the optimal chromatographic separation. In PCR, the concentration data matrix was prepared by using synthetic mixtures containing these drugs in methanol–water (3+1, v/v). The absorbance data matrix corresponding to the concentration data matrix was obtained by measuring the absorbances at 29 wavelengths in the range of 242–298 nm for DIF and ISO in the zero-order spectra of their combinations. In first derivative spectrophotometry, dA/dλ values were measured at 247.8 nm for DIF and at 240.2 nm for ISO in first derivative spectra of the solution of DIF and ISO in methanol–water (3+1, v/v). The linear ranges were 4.00–48.0 μg/mL for DIF and 50.0–400 μg/mL for ISO in the LC method, and 2.40–40.0 μg/mL for DIF and 60.0–260 μg/mL for ISO in the PCR and first derivative spectrophotometric methods. These methods were validated by analyzing synthetic mixtures. These three methods were successfully applied to two pharmaceutical cream preparations.

Optimisation and validation of liquid chromatographic and partial least-squares-1 methods for simultaneous determination of enalapril maleate and nitrendipine in pharmaceutical preparations

2011 ◽  
Vol 65 (6) ◽  
Author(s):  
Mehmet Caglayan ◽  
Ismail Palabiyik ◽  
Mustafa Bor ◽  
Feyyaz Onur
Keyword(s):  
Least Squares ◽  
Simultaneous Determination ◽  
Partial Least Squares ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Data Matrix ◽  
Concentration Data ◽  
Enalapril Maleate ◽  
Nm Range

AbstractSimultaneous determination of enalapril maleate (ENA) and nitrendipine (NIT) in pharmaceutical preparations was performed using liquid chromatography (LC) and the partial least-squares-1 (PLS-1) method. In LC, the separation was achieved on a C8 column and the optimum mobile phase for good separation in a gradient elution programme was found to be acetonitrile-water (φ r = 81: 19) and optimum flow-rate, temperature, injection volume, and detection wavelength were set at 1.0 mL min−1, 25°C, 10 μL, and 210 nm, respectively. Dienogest was selected as an internal standard. In the spectrophotometry, a PLS-1 chemometric method was used. The absorbance data matrix related to the concentration data matrix was established by measurement of absorbances in their zero order spectra with an increment of Δλ = 1 nm in the 220–290 nm range for ENA and with Δλ = 1 nm in the 230–290 nm range for NIT in the PLS-1 method. Following this step, calibration was established by using this data matrix to predict the unknown concentrations of ENA and NIT in their binary mixture. These optimised methods were validated and successfully applied to a pharmaceutical preparation in tablet form and the results were subjected to comparison.

scholarly journals Development and Validation of Spectrophotometric and High-Performance Column Liquid Chromatographic Methods for the Simultaneous Determination of Dienogest and Estradiol Valerate in Pharmaceutical Preparations

2010 ◽  
Vol 93 (3) ◽  
pp. 862-868 ◽  
Author(s):  
Mehmet Gökhan Çağlayan ◽  
Ismail Murat Palabiyik ◽  
Feyyaz Onur
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Pharmaceutical Preparation ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Principal Component ◽  
Data Matrix ◽  
Estradiol Valerate ◽  
Concentration Data

Abstract Simultaneous determination of dienogest (DIE) and estradiol valerate (EST) in sugar-coated tablets was performed by using HPLC and spectrophotometry. In HPLC, the separation was achieved on an ACE C8 column using the mobile phase acetonitrileNH4NO3 (0.03 M, pH 5.4; 70 + 30, v/v) at a flow rate of 2 mL/min. The detection wavelength was 280 nm, and cyproterone acetate was selected as an internal standard. The linearity range was 3.045.0 g/mL for DIE and 18.0100.0 g/mL for EST. As spectrophotometric methods, two chemometric methods, principal component regression and partial least-squares, were developed. In the chemometric techniques, the concentration data matrix was prepared by using mixtures containing these drugs in methanolwater (3 + 1, v/v). The absorbance data matrix corresponding to the concentration data matrix in these methods was obtained by the measurement of absorbances in their zero-order spectra; then, the calibration was obtained by using the data matrix for the prediction of unknown concentrations of DIE and EST in their binary mixture. Working ranges were found as 2.024.0 g/mL for DIE and 20.0270.0 g/mL EST in the methods. These three developed methods were validated and successfully applied to a pharmaceutical preparation, a sugar-coated tablet, and the results were compared with each other.

scholarly journals Multivariate Validated Models for Simultaneous Determination of Ibuprofen and Famotidine in the Presence of Related Substances

2018 ◽  
Vol 101 (4) ◽  
pp. 1001-1007
Author(s):  
Eman S Elzanfaly ◽  
Hala E Zaazaa ◽  
Aya T Soudi ◽  
Maissa Y Salem
Keyword(s):  
Simultaneous Determination ◽  
Multivariate Calibration ◽  
Degradation Products ◽  
Principal Component Regression ◽  
Principal Component ◽  
Standard Addition ◽  
Spectrophotometric Methods ◽  
Related Substances ◽  
Calibration Methods

Abstract Two multivariate validated spectrophotometric methods, namely partial least-squares (PLS) and principal component regression (PCR), were developed and validated for the determination of ibuprofen and famotidine in presence of famotidine degradation products and ibuprofen impurity (4-isobutylacetophenone). A calibration set was prepared in which the two drugs together with the degradation products and impurity were modeled using a multilevel multifactor design. This calibration set was used to build the PLS and PCR models. The proposed models successfully predicted the concentrations of both drugs in validation samples, with low root mean square error of cross validation (RMSECV) percentage. The method was validated by the estimate of the figures of merit depending on the net analyte signal. The results of the two models showed that the simultaneous determination of both drugs could be performed in the concentration ranges of 100–500 µg/mL for ibuprofen and 5–25 µg/mL for famotidine. The proposed multivariate calibration methods were applied for the determination of ibuprofen and famotidine in their pharmaceutical formulation, and the results were verified by the standard addition technique.

Application of independent component analysis, principal component regression and partial least squares methodologies for the simultaneous potentiometric titration of some amino acids

RSC Advances ◽  
2016 ◽  
Vol 6 (74) ◽  
pp. 69902-69908 ◽  
Author(s):  
A. Hakan Aktaş ◽  
Sermin Göksu Karagöz
Keyword(s):  
Amino Acids ◽  
Independent Component Analysis ◽  
Least Squares ◽  
Simultaneous Determination ◽  
Partial Least Squares ◽  
Potentiometric Titration ◽  
Principal Component Regression ◽  
Principal Component ◽  
Chemometric Methods

Potentiometric titration and chemometric methods were applied to the simultaneous determination of the four amino acids, alanine (ALA), phenylalanine (PHE), leucine (LEU) and lysine (LYS).

scholarly journals Universal procedures for spectrophotometric determination of anticoccidial drugs; application to multi-ingredient veterinary formulation and computational investigations for multivariate analysis

2021 ◽  
Vol 12 (4) ◽  
pp. 368-376
Author(s):  
Mahmoud Mohamed Abbas ◽  
Amira Mabrouk El-Kosasy ◽  
Lobna Abd El-Aziz Hussein ◽  
Nancy Magdy Hanna
Keyword(s):  
Multivariate Analysis ◽  
Least Squares ◽  
Simultaneous Determination ◽  
Partial Least Squares ◽  
Principal Component Regression ◽  
Principal Component ◽  
Dual Wavelength ◽  
Ich Guidelines ◽  
The Difference

Simple, accurate, and eco-friendly spectrophotometric procedures were proposed and implemented for simultaneous determination of anticoccidial drugs from three different classes namely, amprolium hydrochloride (AMP), sulfaquinoxaline sodium (SQX) and diaveridine hydrochloride (DVD). Dual wavelength in ratio spectra procedure was proposed where the difference in amplitudes (ΔP) in the ratio spectra at 264 nm and 301.9 nm (ΔP264&301.9 nm) corresponded to AMP with mean percentage recovery 100.00±0.923%, while (ΔP250.9&279 nm) and (ΔP218&243.5 nm) corresponded to SQX and DVD with mean percentage recoveries 99.31±1.083 and 100.64±1.219%, respectively. The dual wavelength in ratio spectra procedure was validated according to the ICH guidelines and accuracy, precision and repeatability were found to be within the acceptable limit. Multivariate chemometric approaches, namely, partial least-squares (PLS-2) and principal component regression (PCR) were also proposed with mean percentage recoveries 99.31±0.769, 98.91±1.192 and 99.04±1.245% for AMP, SQX and DVD, respectively, in PLS-2 and 99.63±1.005, 99.11±1.272 and 98.93±1.338% for AMP, SQX and DVD, respectively, in PCR. These procedures were successfully applied to the multi-ingredient veterinary formulation with mean percentage recoveries 100.75±1.238, 99.29±0.875 and 99.34±0.745% for AMP, SQX and DVD, respectively, in dual wavelength in ratio spectra procedure and 101.03±1.261, 101.48±0.984 and 101.10±1.339% for AMP, SQX and DVD, respectively, in PLS-2 and 100.22±1.204, 101.10±0.546 and 100.91±0.677% for AMP, SQX and DVD, respectively, in PCR.

scholarly journals Application of Derivative, Derivative Ratio, and Multivariate Spectral Analysis and Thin-Layer Chomatography-Densitometry for Determination of a Ternary Mixture Containing Drotaverine Hydrochloride, Caffeine, and Paracetamol

2007 ◽  
Vol 90 (2) ◽  
pp. 391-404 ◽  
Author(s):  
Fadia H Metwally ◽  
Yasser S El-Saharty ◽  
Mohamed Refaat ◽  
Sonia Z El-Khateeb
Keyword(s):  
Thin Layer ◽  
Least Squares ◽  
Ternary Mixture ◽  
Principal Component Regression ◽  
Pharmaceutical Preparations ◽  
Principal Component ◽  
Standard Addition ◽  
Drotaverine Hydrochloride ◽  
Assay Precision

Abstract New selective, precise, and accurate methods are described for the determination of a ternary mixture containing drotaverine hydrochloride (I), caffeine (II), and paracetamol (III). The first method uses the first (D1) and third (D3) derivative spectrophotometry at 331 and 315 nm for the determination of (I) and (III), respectively, without interference from (II). The second method depends on the simultaneous use of the first derivative of the ratio spectra (DD1) with measurement at 312.4 nm for determination of (I) using the spectrum of 40 μg/mL (III) as a divisor or measurement at 286.4 and 304 nm after using the spectrum of 4 μg/mL (I) as a divisor for the determination of (II) and (III), respectively. In the third method, the predictive abilities of the classical least-squares, principal component regression, and partial least-squares were examined for the simultaneous determination of the ternary mixture. The last method depends on thin-layer chromatography-densitometry after separation of the mixture on silica gel plates using ethyl acetatechloroformmethanol (16 + 3 + 1, v/v/v) as the mobile phase. The spots were scanned at 281, 272, and 248 nm for the determination of (I), (II), and (III), respectively. Regression analysis showed good correlation in the selected ranges with excellent percentage recoveries. The chemical variables affecting the analytical performance of the methodology were studied and optimized. The methods showed no significant interferences from excipients. Intraday and interday assay precision and accuracy values were within regulatory limits. The suggested procedures were checked using laboratory-prepared mixtures and were successfully applied for the analysis of their pharmaceutical preparations. The validity of the proposed methods was further assessed by applying a standard addition technique. The results obtained by applying the proposed methods were statistically analyzed and compared with those obtained by the manufacturer's method.

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