APPLICATION OF CHEMOMETRIC METHODS FOR DETERMINATION OF CLOTRIMAZOLE AND BECLOMETHASONE DIPROPIONATE IN PHARMACEUTICAL DOSAGE FORM

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.

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.


2019 ◽  
Vol 2019 ◽  
pp. 1-8
Author(s):  
Guzide Pekcan Ertokus

The spectrophotometric-chemometric analysis of levodopa and carbidopa that are used for Parkinson’s disease was analyzed without any prior reservation. Parkinson’s drugs in the urine sample of a healthy person (never used drugs in his life) were analyzed at the same time spectrophotometrically. The chemometric methods used were partial least squares regression (PLS) and principal component regression (PCR). PLS and PCR were successfully applied as chemometric determination of levodopa and carbidopa in human urine samples. A concentration set including binary mixtures of levodopa and carbidopa in 15 different combinations was randomly prepared in acetate buffer (pH 3.5).). UV spectrophotometry is a relatively inexpensive, reliable, and less time-consuming method. Minitab program was used for absorbance and concentration values. The normalization values for each active substance were good (r2>0.9997). Additionally, experimental data were validated statistically. The results of the analyses of the results revealed high recoveries and low standard deviations. Hence, the results encouraged us to apply the method to drug analysis. The proposed methods are highly sensitive and precise, and therefore they were implemented for the determination of the active substances in the urine sample of a healthy person in triumph.


2008 ◽  
Vol 59 (2) ◽  
pp. 154-158 ◽  
Author(s):  
Gozde Pektas ◽  
Erdal Dinc ◽  
Dumitru Baleanu

Principal component regression (PCR) and partial least squares (PLS) chemometric methods were applied to the simultaneous quantitative analysis of levamisole (LVM) and triclabendazole (TCB) in tablets without using a preliminary separation, even in presence of the overlapping spectra of the above compounds. For both PCR and PLS, a concentration set containing 25 different mixtures of LVM and TCB in the linear concentration range was symmetrically prepared and then the absorbance values of the concentration set were measured at the wavelength set with Dl=0.1 nm in the spectral region of 225-322.3 nm. PCR and PLS calibrations were obtained by applying the PCR and PLS algorithms to the concentration set data (y-block) and their corresponding absorbance data (x-block). The validity of PCR and PLS chemometric methods was performed by using the independent synthetic mixtures and the standard addition technique. Then, these analytical methods were applied to the commercial tablets and a good agreement was obtained between experimental results provided by the application of the PCR and PLS to the synthetic and real samples.


2018 ◽  
Vol 101 (2) ◽  
pp. 394-400 ◽  
Author(s):  
Khalid A M Attia ◽  
Nasr M El-Abasawi ◽  
Ahmed El-Olemy ◽  
Ahmed H Abdelazim

Abstract Three UV spectrophotometric methods have been developed for the simultaneous determination of two new Food and Drug Administration-approved drugs, elbasvir (EBV) and grazoprevir (GRV), in their combined pharmaceutical dosage form. These methods include dual wavelength (DW), classic least-squares (CLS), and principal component regression (PCR). To achieve the DW method, two wavelengths were chosen for each drug in a way to ensure the difference in absorbance was zero from one drug to the other. GRV revealed equal absorbance at 351 and 315 nm, for which the distinctions in absorbance were measured for the determination of EBV. In the same way, distinctions in absorbance at 375 and 334.5 nm were measured for the determination of GRV. Alternatively, the CLS and PCR models were applied to the spectra analysis because the synchronous inclusion of many unreal wavelengths rather than using a single wavelength greatly increased the precision and predictive ability of the methods. The proposed methods were successfully applied to the assay of these drugs in their pharmaceutical formulation. The obtained results were statistically compared with manufacturing methods. The results conclude that there was no significant difference between the proposed methods and the manufacturing method with respect to accuracy and precision.


2005 ◽  
Vol 88 (4) ◽  
pp. 1069-1080 ◽  
Author(s):  
Alaa El-Gindy ◽  
Samy Emara ◽  
Mostafa K Mesbah ◽  
Ghada M Hadad

Abstract Three methods were applied for the analysis of 2 multicomponent mixtures containing dextromethorphan hydrobromide, phenylephrine hydrochloride, chlorpheniramine maleate, methylparaben, and propylparaben, together with either sodium benzoate (Mix 1) or ephedrine hydrochloride and benzoic acid (Mix 2). In the first method, liquid chromatography was used for their simultaneous determination using an ODS column with a mobile phase consisting of acetonitrile–phosphate buffer, pH 2.7 (40 + 60, v/v), containing 5mM heptanesulfonic acid sodium salt and ultraviolet (UV) detection at 214 nm. Also, 2 chemometric methods, principal component regression, and partial least squares were used. For both chemometric calibrations, a concentration set of the mixture consisting of each compound in each mixture was prepared in distilled water. The absorbance data in the UV spectra were measured for the 76 or 71 wavelength points in the spectral region 210–240 or 210–224 nm considering the intervals of Δλ = 0.4 or 0.2 nm for Mix 1 and Mix 2, respectively. The 2 chemometric methods did not require any separation step. These methods were successfully applied for the analysis of the 2 multicomponent combinations in synthetic mixtures and in commercial syrups, and the results were compared with each other.


2005 ◽  
Vol 88 (4) ◽  
pp. 1126-1134 ◽  
Author(s):  
Khadiga M Kelani

Abstract A ratio-spectra zero-crossing first-derivative spectrophotometric method and 2 chemometric methods have been used for the simultaneous determination of ternary mixtures of caffeine (A), 8-chlorotheophylline (B), and chlorphenoxamine hydrochloride (C) in bulk powder and dosage forms. In the ratio-spectra zero-crossing first-derivative spectrophotometric technique (1DD), calibration curves were linear in the range of 4–20 μg/mL for A, B, and C (r = 0.9992, 0.9994, and 0.9976, respectively). The measurements were carried out at 212, 209.2, and 231.4 nm for A, B, and C, respectively. The detection limits for A, B, and C were calculated to be 0.24, 0.34, and 0.13 μg/mL, and the percentage recoveries were 99.1 ± 0.89, 100.1 ± 0.95, and 100.1 ± 1.0, respectively. Two chemometric methods, namely, the partial least-squares (PLS) model and the principal component regression (PCR) model, were also used for the simultaneous determination of the 3 drugs in the ternary mixture. A training set consisting of 15 mixtures containing different ratios of A, B, and C was used. The concentration used for the construction of the PLS and PCR models varied between 4 and 25 μg/mL for each drug. These models were used after their validation for the prediction of the concentrations of A, B, and C in mixtures. The detection limits for A, B, and C were calculated to be 0.13, 0.15, and 0.14 μg/mL, respectively, and the percent recoveries were found to be 99.8 ± 0.96, 99.9 ± 0.94, and 99.9 ± 1.18, respectively, for both methods. The 3 proposed procedures are rapid, simple, sensitive, and accurate. No preliminary separation steps or resolution equations are required; thus, they can be applied to the simultaneous determination of the 3 drugs in commercial tablets and suppositories or in quality-control laboratories.


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%).


2016 ◽  
Vol 99 (4) ◽  
pp. 941-947
Author(s):  
Omar Abdel-Aziz ◽  
Emad M Hussien ◽  
Amira M El Kosasy ◽  
Neven Ahmed

Abstract Six simple, accurate, reproducible, and selective derivative spectrophotometric and chemometric methods have been developed and validated for the determination of levamisole HCl (Lev) either alone or in combination with closantel sodium (Clo) in the pharmaceutical dosage form. Lev was determined by first-derivative, first-derivative ratio, and mean-centering methods by measuring the peak amplitude at 220.8, 243.8, and 210.4 nm, respectively. The methods were linear over the concentration range 2.0–10.0 μg/mL Lev. The methods exhibited a high accuracy, with recovery data within ±1.9% and RSD &lt;1.3% (n = 9) for the determination of Lev in the presence of Clo. Fortunately, Lev showed no significant UV absorbance at 370.6 nm, which allowed the determination of Clo over the concentration range 16.0–80.0 μg/mL using zero-order spectra, with a high precision (RSD &lt;1.5%, n = 9). Furthermore, principal component regression and partial least-squares with optimized parameters were used for the determination of Lev in the presence of Clo. The recovery was within ±1%, with RSD &lt;1.0% (n = 9) and root mean square error of prediction ≤1.0. The proposed methods were validated according to the International Conference on Harmonization guidelines. The proposed methods were used in the determination of Lev and Clo in a binary mixture and a pharmaceutical formulation, with high accuracy and precision.


Processes ◽  
2021 ◽  
Vol 9 (8) ◽  
pp. 1272
Author(s):  
Seetharaman Rathinam ◽  
Lakshmi Karunanidhi Santhana

This work introduces three eco-friendly UV spectrophotometric methods for the simultaneous estimation of Paracetamol, Aceclofenac and Eperisone Hydrochloride in pharmaceutical tablet formulation. The procedures employed were simultaneous equation method and multivariate chemometric methods with phosphate buffer pH 7.80 as diluent. The simultaneous equation method encompasses absorbance measurement at three different wavelengths (λmax of the drugs). It exhibits linearity between 12–18 µg mL−1 for paracetamol, 3.69–5.53 µg mL−1 for Aceclofenac, and 2.76–4.15 µg mL−1 Eperisone hydrochloride. The results obtained for accuracy and precision by the simultaneous equation method were within the permissible limits. Principal component regression and partial least squares were the tools used for chemometric methods. The calibration set and prediction set were constructed, and the UV spectra were recorded in zero order mode, further subjected to chemometric analysis. The % recoveries obtained for Paracetamol, Aceclofenac, and Eperisone Hydrochloride by chemometric techniques showed good accuracy, and the results obtained for analytical figures of merit were acceptable. Statistical comparison of the assay results obtained for the proposed methods showed no significant difference found among the methods using one way analysis of variance. Greenness evaluation tools revealed the greenness profile of the proposed methods and found them to be ecofriendly. The described methods were appropriate for routine quality control laboratories, facilitating eco-friendly, fast, and cost effective determination of Paracetamol, Aceclofenac, and Eperisone Hydrochloride in Acemyoset P tablets.


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