scholarly journals Simultaneous Determination of Chlorthalidone and Spironolactone with Univariate and Multivariate Calibration: Wavelength Range Selection

1999 ◽  
Vol 82 (5) ◽  
pp. 1054-1063 ◽  
Author(s):  
M Luz Luis ◽  
José M García ◽  
Francisco Jiménez ◽  
Ana I Jiménez ◽  
Juan J Arias

Abstract Chlorthalidone and spironolactone were determined simultaneously with the aid of univariate and multivariate calibration methods. Univariate calibration was performed by the zero-crossing and derivative ratio spectrum methods. Extensive spectral overlap and the scarcity of wavelengths in derivative spectra allowing one analyte to be distinguished and quantitated in the presence of the other gave rise to poor results that called for multivariate calibration. Partial least-squares regression was used in combination with a suitable method for selecting the optimum wavelength range and number of factors for analysis. The ensuing method was applied to simultaneous determination of chlorthalidone and spironolactone in a commercially available pharmaceutical preparation. The results were validated by high-performance liquid chromatography.

2020 ◽  
Vol 16 ◽  
Author(s):  
Abdürrezzak E. Bozdoğana ◽  
Özlem Aksu Dönmez ◽  
Şule Dinç-Zor

Introduction: This study introduces an effective strategy which combines high performance liquid chromatography coupled with diode array detection (HPLC-DAD) with multivariate calibration methods for the simultaneous determination paracetamol (PAR), pseudoephedrine HCl (PSE), dextromethorphan HBr (DEX) and doxylamine succinate (DOX) along with sweetener saccharine (SAC) in syrup formulation. Methods: PLS-2 and PCR calibration algorithms were selected for data processing. Based on the strategy, all target analytes were rapidly quantified within 5.3 min under the simple isocratic elution (water : methanol, 20/80, v/v) without a complete separation. The performances of the proposed methods were confirmed by analyzing a series of synthetic solutions including different concentrations of analytes Results: The average recovery values were in the range of 100.33 to 103.70%, and the REP (relative error of prediction) values ranged from 1.96 to 4.36% showed that these methods could provide satisfactory predictions. Conclusion: Novel HPLC methods coupled with PLS and PCR algorithm enable a simple, fast and low-cost analysis of similar pharmaceutical products for simultaneous determination of the target compounds.


2018 ◽  
Vol 101 (2) ◽  
pp. 414-426 ◽  
Author(s):  
Azza A Moustafa ◽  
Maha A Hegazy ◽  
Dalia Mohamed ◽  
Omnia Ali

Abstract The presence of coloring matters in syrups usually interferes with the spectrophotometric determination of active pharmaceutical ingredients. A novel approach was introduced to eliminate the interference of sunset yellow (coloring matter) in Cyrinol syrup. Smart, simple, accurate, and selective spectrophotometric methods were developed and validated for the simultaneous determination of a ternary mixture of carbinoxamine maleate, pholcodine, and ephedrine hydrochloride in syrup. Four of the applied methods used ratio spectra: successive derivative subtraction coupled with constant multiplication, successive derivative of ratio spectra, ratio subtraction coupled with ratio difference, and ratio spectra continuous wavelet transforms zero-crossing. In addition, a method that was based on the presence of an isosbestic point, the amplitude summation method, was also established. A major advantage of the proposed methods is the simultaneous determination of the mentioned drugs without prior separation steps. These methods were successfully applied for the determination of laboratory-prepared mixtures and a commercial pharmaceutical preparation without interference from additives, thus proving the selectivity of the methods. No significant difference regarding both accuracy and precision was observed upon statistical comparison of the results obtained by the proposed methods with each other and with those of official or reported ones.


2000 ◽  
Vol 405 (1-2) ◽  
pp. 153-160 ◽  
Author(s):  
Javier Saurina ◽  
Santiago Hernández-Cassou ◽  
Esteve Fàbregas ◽  
Salvador Alegret

2008 ◽  
Vol 73 (2) ◽  
pp. 233-247 ◽  
Author(s):  
Mohammad Karimi ◽  
Mazloum Ardakani ◽  
Reza Behjatmanesh-Ardakani ◽  
Hormozi Nezhad ◽  
Hamzeh Amiryan

Individual and simultaneous determinations of some phenothiazine drugs are described. The individual determination method is based on the reaction of chlorpromazine hydrochloride (CPH), promethazine hydrochloride (PH), trifluoperazine hydrochloride (TFPH), trimipramine maleate (TPM) and thioridazine hydrochloride (TRDH) with complex of [Fe(Bpy)3]3+. In the presence of phenothiazine derivatives, [Fe(Bpy)3]3+ is reduced easily to the colored complex [Fe(Bpy)3]2+, which shows an absorption maximum at 525 nm. The individual method is highly sensitive and suitable for 0.3-190 ?g ml-1 concentrations, with detection limits in the range 0.18-2.46 ?g ml-1. Simultaneous kinetic-spectrophotometric determination of ternary mixture of CPH, PH and TPM using principal component regression (PCR), partial least squares (PLS) and orthogonal signal correction (OSC)-PLS multivariate calibration methods is also described. The simultaneous methods are based on the difference observed in the reduction rate of the [Fe(Bpy)3]3+ complex with CPH, PH and TPM in acidic media. The results showed that the simultaneous determination of CPH, PH and TPM can be performed in the concentration ranges of 0.5-120.0, 0.3-80.0 and 5.0-100.0 ?g ml-1, respectively, for three methods (PCR, PLS and OSC-PLS). The root mean square errors of prediction (RMSEP) of CPH, PH and TPM were 0.346, 0.663 and 0.820 (for PCR) 0.317, 0.659 and 0.830 (for PLS) and 0.087, 0.124 and 0.085 (for OSC-PLS), respectively. The proposed methods were successfully applied to the individual and simultaneous determination of phenothiazine derivatives in pharmaceutical preparations, the results of which compared well with those obtained by the official method, and several synthetic (spiked) samples, whereby satisfactory results were obtained.


2010 ◽  
Vol 93 (3) ◽  
pp. 862-868 ◽  
Author(s):  
Mehmet Gökhan Çağlayan ◽  
Ismail Murat Palabiyik ◽  
Feyyaz Onur

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.


2009 ◽  
Vol 92 (1) ◽  
pp. 119-124 ◽  
Author(s):  
Azzam R Ali ◽  
Ibrahim I Duraidi ◽  
Munib M Saket ◽  
Eyad S M Abu-Nameh

Abstract An efficient, sensitive, and simple method was developed for the simultaneous determination of rosiglitazone and metformin hydrochloride in a combination tablet dosage form by column high-performance liquid chromatography. The mobile phase used was ammonium dihydrogen phosphate adjusted to pH 5.25 with sodium hydroxide. The limits of detection and quantitation were in the range of 0.51.6 g/mL, respectively, for metformin hydrochloride, and 0.002010.0067 g/mL, respectively, for rosiglitazone. The linearity was studied in the concentration range of 0.120.31 g/mL for rosiglitazone and 30.676.7 g/mL for metformin hydrochloride. The recovered amounts of metformin hydrochloride and rosiglitazone were 100103.8 and 101103.7, respectively.


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