scholarly journals Chemometric-Assisted Spectrophotometric Method for the Simultaneous Determination of Ciprofloxacin and Doxycycline Hyclate in Pharmaceutical Formulations

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%).

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.


2016 ◽  
Vol 51 (4) ◽  
pp. 297-306 ◽  
Author(s):  
SS Israt ◽  
MN Uddin ◽  
RA Jahan ◽  
MM Karim

The combination of furosemide (furo) and spironolactone (spiro) is very effective in the treatment of heart failure. In that case, maintaining good quality of these drugs in commercial tablets is must. Therefore, a simple, economical, precise and accurate method, i.e; chemometric assisted UV spectroscopy, for simultaneous determination of furosemide and spironolactone in combined dosage form has been developed. In this study, principal component regression (PCR) has been reported for this purpose. A calibration set of 36 mixture solutions containing furosemide and spironolactone in methanol in the concentration range of 2.0-12.0 ?g/ml and 5.0-30.0 ?g/ml respectively has been prepared by means of an orthogonal experimental design. The absorbance data for the concentration set have been obtained by direct measurement in UV spectrophotometer at 101 wavelength points in the spectral region of 200-300 nm for the zero order spectra. The chemometric technique is also successfully applied to available pharmaceutical formulations, tablets, with no interference from excipients. The analytical performances of principal component regression are characterized by relative prediction errors and recoveries (%). The good recoveries obtained in this case proved that the proposed chemometric technique could be applied efficiently in the quality control of the studied drugs simultaneously in their mixture as well as in the commercial dosage form with satisfactory precision and accuracy as alternative analysis tools.Bangladesh J. Sci. Ind. Res. 51(4), 297-306, 2016


2011 ◽  
Vol 94 (5) ◽  
pp. 1427-1439
Author(s):  
Samah S Abbas ◽  
Nour E Wagieh ◽  
Mohamed Abdelkawy ◽  
Maha M Abdelrahman

Abstract Three methods are presented for the simultaneous determination of diloxanide furoate (DLX) and metronidazole (MTR), used for their antiprotozoal and antiamoebic effect, in the presence of DLX alkaline degradates and in pharmaceutical formulations, without previous separation. The first method is chemometric-assisted spectrophotometry, in which principal component regression and partial least squares were applied. These two approaches were successfully applied to quantify each drug in the mixture using the information included in the absorption spectra in the range of 225–320 nm. The second method is TLC-densitometry, in which the binary mixture and degradates were separated on silica gel plates using a chloroform–acetone–glacial acetic acid (9.5 + 0.5 + 0.07, v/v/v) mobile phase and the bands were scanned at 254 nm. The last method is HPLC, in which DLX, MTR, and degradates were separated using the mobile phase acetonitrile–0.05 M dibasic potassium phosphate (25 + 75, v/v), adjusted to pH 4 with orthophosphoric acid, at a flow rate of 1 mL/min, on a C18 analytical column. Detection was at 254 nm. The proposed methods were successfully applied for the analysis of DLX and MTR in pharmaceutical formulations, and the results were statistically compared with a reported spectrophotometric method.


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.


2020 ◽  
Vol 103 (1) ◽  
pp. 250-256 ◽  
Author(s):  
Shereen A Boltia ◽  
Aya T Soudi ◽  
Eman S Elzanfaly ◽  
Hala E Zaazaa

Abstract Background: The utilization of selection methods such as genetic algorithm (GA) aims to construct better partial least squares (PLS) and principal component regression (PCR) models than those established from the full-spectrum range. Objective: Determination of paracetamol (PAR), orphenadrine citrate (Or.cit), and caffeine (CAF) in the presence of PAR nephrotoxic impurity [p-aminophenol (PAP)]. GA was applied to select the optimum wavelengths used. Methods: A calibration set was prepared in which the three drugs, together with PAP, were modeled by multilevel multifactor design. This calibration set was used to build the PLS and PCR models, either with or without preprocessing the data using GA. Results: Results were compared with and without preprocessing, and this revealed that GA can find an optimized combination of spectral wavelengths, yielding a lower root mean square error of prediction as well as a lower number of latent variables used. The results of the two models show that simultaneous determination of the aforementioned drugs can be performed in the concentration ranges of 20–60, 3–11, and 1–9 μg/mL for PAR, Or.cit, and CAF, respectively. Conclusions: The proposed models were applied for the determination of the three drugs in their pharmaceutical formulations, and the results were verified by the standard addition technique. Highlights: GA can be useful as a wavelength selection tool before applying multivariate PLS and PCR methods. GA gives an improvement in the predictive ability of the models with lower RMSEP and less number of latent variables (LVs). The proposed PLS, PCR, GA-PLS, and GA-PCR spectrophotometric methods were able to determine paracetamol, orphenadrine citrate, and caffeine in the presence of p-aminophenol and severe spectral overlapping.


2014 ◽  
Vol 1060 ◽  
pp. 164-167
Author(s):  
Lawan Sratthaphut ◽  
Kanong Ruttanakorn

This study aims to estimate simultaneously metformin hydrochloride (MET) and glyburide (GLY) in a multicomponent tablets dosage form by spectrophotometric method using chemometric approaches such as principal component regression (PCR) and partial least-squares regression (PLS). Because of highly overlapped in UV spectra and difference proportions of two active ingredients, the conventional univariate calibration methods was not allowed without previous separation. The linearity ranges used to construct the calibration matrix were selected in the ranges from 40.00 to 200.00 mg L-1for MET and from 1.00 to 10.00 mg L-1for GLY. The absorbances were measured in the wavelength range of 200-400 nm, using ethanol as solvent. The resulting UV spectra were subjected to PCR and PLS algorithms and the optimum numbers of principal components (PCs) were selected according to prediction residual error sum of squares (PRESS) values of leave-one out cross-validation. The number of PCs for MET and GLY were found to be 5, 3 by PCR and 5, 3 by PLS, respectively. A set of synthetic mixtures was employed to verify the models and the performance of the models were shown in the values of the root mean square error in prediction (RMSEP). RMSEP values of MET and GLY were 1.806, 0.256 for PCR and 1.802, 0.185 for PLS, respectively. The suitable calibration models were applied to the analysis of these compounds in pharmaceutical formulation.


2012 ◽  
Vol 622-623 ◽  
pp. 1451-1455
Author(s):  
Qiang Deng ◽  
Long Jiao ◽  
Yi Qing Ge ◽  
Yun Xia Wang

A method which combines UV spectroscopy, guest–host chemistry and principal component regression (PCR) was proposed for determining the enantiomeric composition of DOPA samples. The calibration models were developed from UV spectral data of a series of samples containing DOPA with different known enantiomeric compositions by using PCR. The obtained model was subsequently validated by determining the enantiomeric composition of a set of independently prepared samples. This method shows high sensitivity for determining the enantiomeric composition of DOPA. When there is 5.00 μM DOPA in the samples, the enantiomeric composition of DOPA can be accurately determined.


2007 ◽  
Vol 90 (2) ◽  
pp. 391-404 ◽  
Author(s):  
Fadia H Metwally ◽  
Yasser S El-Saharty ◽  
Mohamed Refaat ◽  
Sonia Z El-Khateeb

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.


2021 ◽  
Vol 19 (1) ◽  
pp. 205-213
Author(s):  
Hany W. Darwish ◽  
Abdulrahman A. Al Majed ◽  
Ibrahim A. Al-Suwaidan ◽  
Ibrahim A. Darwish ◽  
Ahmed H. Bakheit ◽  
...  

Abstract Five various chemometric methods were established for the simultaneous determination of azilsartan medoxomil (AZM) and chlorthalidone in the presence of azilsartan which is the core impurity of AZM. The full spectrum-based chemometric techniques, namely partial least squares (PLS), principal component regression, and artificial neural networks (ANN), were among the applied methods. Besides, the ANN and PLS were the other two methods that were extended by genetic algorithm procedure (GA-PLS and GA-ANN) as a wavelength selection procedure. The models were developed by applying a multilevel multifactor experimental design. The predictive power of the suggested models was evaluated through a validation set containing nine mixtures with different ratios of the three analytes. For the analysis of Edarbyclor® tablets, all the proposed procedures were applied and the best results were achieved in the case of ANN, GA-ANN, and GA-PLS methods. The findings of the three methods were revealed as the quantitative tool for the analysis of the three components without any intrusion from the co-formulated excipient and without prior separation procedures. Moreover, the GA impact on strengthening the predictive power of ANN- and PLS-based models was also highlighted.


2015 ◽  
Vol 4 (4) ◽  
pp. 378-381 ◽  
Author(s):  
Mannem Sri Varsha ◽  
N. Raghavendra Babu ◽  
Yenumula Padmavathi ◽  
P. Ravi Kumar

A new simple, sensitive and specific procedure has been developed for determination of tenofovir disoproxil fumarate in bulk and pharmaceutical dosage forms using MBTH reagent. The purpose of this analytical validation procedure is to validate it by laboratory experiments to prove that the method meets the minimum standards for laboratory use. 3-methyl-2-bezothiazoline hydrazone reacts with the secondary amine group of tenofovir in the presence of oxidizing agent, ferric chloride. The resulting apple green coloured chromogen when measured spectrophotometrically in visible region (i.e., 400-800nm) shows a maximum absorbance at 626.5nm. This method can be successfully applied for the determination of drug content in pharmaceutical formulations. The results of analysis have been validated statistically.DOI: http://dx.doi.org/10.3329/icpj.v4i4.22620 International Current Pharmaceutical Journal, March 2015, 4(4): 378-381 


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