scholarly journals Novel Stability-Indicating Chemometric-Assisted Spectrophotometric Methods for the Determination of Chlordiazepoxide and Clidinium Bromide in the Presence of Clidinium Bromide’s Alkali-Induced Degradation Product

2018 ◽  
Vol 101 (3) ◽  
pp. 714-722 ◽  
Author(s):  
Christine K Nessim ◽  
Adel M Michael ◽  
Yasmin M Fayez ◽  
Hayam M Lotfy

Abstract Two simple and accurate chemometric-assisted spectrophotometric models were developed and validated for the simultaneous determination of chlordiazepoxide (CDZ) and clidinium bromide (CDB) in the presence of an alkali-induced degradation product of CDB in their pure and pharmaceutical formulation. Resolution was accomplished by using two multivariate calibration models, including principal component regression (PCR) and partial least-squares (PLS), applied to the UV spectra of the mixtures. Great improvement in the predictive abilities of these multivariate calibrations was observed. A calibration set was constructed and the best model used to predict the concentrations of the studied drugs. CDZ and CDB were analyzed with mean accuracies of 99.84 ± 1.41 and 99.81 ± 0.89% for CDZ and 99.56 ± 1.43 and 99.44 ± 1.41% for CDB using PLS and PCR models, respectively. The proposed models were validated and applied for the analysis of a commercial formulation and laboratory-prepared mixtures. The developed models were statistically compared with those of the official and reported methods with no significant differences observed. The models can be used for the routine analysis of both drugs in QC laboratories.

2018 ◽  
Vol 101 (4) ◽  
pp. 1001-1007
Author(s):  
Eman S Elzanfaly ◽  
Hala E Zaazaa ◽  
Aya T Soudi ◽  
Maissa Y Salem

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.


2018 ◽  
Vol 2018 ◽  
pp. 1-5 ◽  
Author(s):  
Tadele Eticha ◽  
Getu Kahsay ◽  
Fitsum Asefa ◽  
Teklebrhan Hailu ◽  
Hailekiros Gebretsadik ◽  
...  

Two chemometrics methods—principal component regression and partial least squares—were developed for simultaneous spectrophotometric estimation of ciprofloxacin and doxycycline hyclate in pharmaceutical dosage forms without any pretreatment. The UV spectra of both drugs were recorded at concentrations within their linear ranges between 200 and 400 nm with the intervalsλ= 2 nm at 100 wavelengths in distilled water. Beer’s law was obeyed for both drugs in the concentration ranges of 1–10 μg/mL for ciprofloxacin and 5–25 μg/mL for doxycycline hyclate. Two sets of standard mixtures, 25 as a calibration set and 9 as a validation set, were prepared. The calibration models were evaluated by cross-validation and external validation over synthetic mixtures. The optimized models were successfully applied for chemometric analysis of ciprofloxacin and doxycycline hyclate in synthetic and pharmaceutical mixtures with satisfactory accuracy (recovery values from 97.50% to 101.87%) and precision (RSD < 2%).


1992 ◽  
Vol 46 (11) ◽  
pp. 1685-1694 ◽  
Author(s):  
Tomas Isaksson ◽  
Charles E. Miller ◽  
Tormod Næs

In this work, the abilities of near-infrared diffuse reflectance (NIR) and transmittance (NIT) spectroscopy to noninvasively determine the protein, fat, and water contents of plastic-wrapped homogenized meat are evaluated. One hundred homogenized beef samples, ranging from 1 to 23% fat, wrapped in polyamide/polyethylene laminates, were used. Results of multivariate calibration and prediction for protein, fat, and water contents are presented. The optimal test set prediction errors (root mean square error of prediction, RMSEP), obtained with the use of the principal component regression method with NIR data, were 0.45, 0.29 and 0.50 weight % for protein, fat, and water, respectively, for plastic-wrapped meat (compared to 0.40, 0.28 and 0.45 wt % for unwrapped meat). The optimal prediction errors for the NIT method were 0.31, 0.52 and 0.42 wt % for protein, fat, and water, respectively, for plastic-wrapped meat samples (compared to 0.27, 0.38, and 0.37 wt % for unwrapped meat). We can conclude that the addition of the laminate only slightly reduced the abilities of the NIR and NIT method to predict protein, fat, and water contents in homogenized meat.


2016 ◽  
Vol 99 (5) ◽  
pp. 1247-1251 ◽  
Author(s):  
Hamed M Elfatatry ◽  
Mokhtar M Mabrouk ◽  
Sherin F Hammad ◽  
Fotouh R Mansour ◽  
Amira H Kamal ◽  
...  

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.


2011 ◽  
Vol 94 (1) ◽  
pp. 128-135 ◽  
Author(s):  
Elif Karacan ◽  
Mehmet Gokhan Çaġlayan ◽  
İsmail Murat Palabiyik ◽  
Feyyaz Onur

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.


The Analyst ◽  
1994 ◽  
Vol 119 (7) ◽  
pp. 1537-1540 ◽  
Author(s):  
Mercedes Jiménez Arrabal ◽  
Pablo Valiente González ◽  
Concepción Caro Gámez ◽  
Antonio Sánchez Misiego ◽  
Arsenio Muñoz de la Peña

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (02) ◽  
pp. 45-50
Author(s):  
Umang Shah ◽  
Bhumika Desai ◽  
Vyomesh Nandrubarkar

Chemometry is the use of mathematical and statistical methods to improve the understanding of chemical information and to correlate quality parameters or physical properties to analytical instrument data. In the present work, two chemometric methods, named as principal component regression (PCR) and (PLS) based on the use of spectrophotometric data, were developed for simultaneous determination of clotrimazole (CLO) and beclomethasone dipropionate (BE C) in bulk and cream form. The absorbance of zero order UV spectra of CLO and BE C in the range of 80-400 μg/mL and 2-10 μg/mL, respectively were recorded in the wavelength range 230-272 nm at 3 nm wavelength intervals. Twenty-five (25) mixed solutions were prepared for the chemometric calibration as training set and sixteen varied solutions were prepared as a validation set. The suitability of the models was decided based on the RMSECV, RMSEP and PRESS values of calibration and validation data. The % recovery study of both the methods was compared, and it was found near each other. The assay of CLO and BE C for both the methods was found to be in the range of 99.78 to 101.20%. Hence, the proposed methods can be used for simultaneous analysis of the mixture of the drugs, without chemical pre-treatment, with good speed of analysis.


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