SIMULTANEOUS ESTIMATION OF DAPAGLIFOZIN AND SAXAGLIPTIN IN TABLETS USING TWO CHEMOMETRIC-ASSISTED UV-SPECTROPHOTOMETRIC METHODS

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (03) ◽  
pp. 32-38
Author(s):  
S. S Sonawane ◽  
S. S More ◽  
S. S. Chhajed ◽  
S. J. Kshirsagar ◽  

Two simple, accurate, precise and economical UV spectrophotometric methods, Multiple Linear Regression (MLR) and Principal Component Regression (PCR), were developed for the simultaneous estimation of dapaglifozin (DAPA) and saxagliptin (SAXA) in tablets. Beer’s law was obeyed in the concentration ranges of 10 – 50 μg/mL for DAPA and 5 – 25 μg/mL for SAXA. Synthetic mixtures containing two drugs were prepared to build the training set and validation set in the calibration range using D-optimal mixture design in phosphate buffer pH 6.8 and were recorded at six wavelengths in the range of 230 – 215 nm at intervals of Δλ = 3 nm. Both methods were validated as per ICH guidelines with respect to the accuracy and precision and found suitable for routine analysis of tablets containing DAPA and SAXA without separation.

2019 ◽  
Vol 16 (1) ◽  
pp. 64-84
Author(s):  
Maissa Yacuob Salem ◽  
Nagiba Yehia Hassan ◽  
Yasmin Mohamed Fayez ◽  
Samah Abd ElSabour ◽  
Enas Shaaban Ali

Background: Hydrochlorothiazide (HCTZ) is potent diuretic that is used alone or in combination with other drugs such as labetalol (Lab) (mixtures Ι) or nebivolol (Neb) (mixtures ΙΙ) to control moderate to sever hypertension. Introduction: This paper demonstrates the establishment of different validated spectrophotometric and chemometric methods for simultaneous estimation of these mixtures in pure form and pharmaceutical formulations in the presence of HCTZ related impurities in quality control laboratories. Methods: (A) Derivative method (D3) of Lab and HCTZ and its related impurities at 245.3nm and 278.5nm respectively, (D1) of Neb and HCTZ at 294.2nm and 282.2nm, respectively. (B) First derivative of ratio spectra method (DD 1) of Lab at 244.3nm, HCTZ at 261.2nm and 275.4nm, while at 294nm for Neb and 269.4nm for HCTZ. (C) Ratio difference method which depends on measuring the distinction between the amplitudes of ratio spectra at 240nm and 288.3nm for Lab and at 270.1nm and 277.4nm for HCTZ for mixture Ι while at 290.4nm and 299.2nm for Neb and at 232.2nm and 254nm for HCTZ for mixture ΙΙ. (D) Mean centering of ratio spectra (MC) and (E) partial least squares regression (PLS) and principal component regression (PCR). Results: These methods were applied over concentration ranges of 10-100 µg/ml, 10-75 µg/ml and 2.5- 25 µg/ml of Lab, Neb and HCTZ, respectively. Methods were validated according to ICH guidelines and statistical comparison of results of reported and proposed methods revealed no difference. Conclusion: The methods were successfully used for the frequent analysis of selected mixtures in quality control laboratories.


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.


Author(s):  
Hervé Cardot ◽  
Pascal Sarda

This article presents a selected bibliography on functional linear regression (FLR) and highlights the key contributions from both applied and theoretical points of view. It first defines FLR in the case of a scalar response and shows how its modelization can also be extended to the case of a functional response. It then considers two kinds of estimation procedures for this slope parameter: projection-based estimators in which regularization is performed through dimension reduction, such as functional principal component regression, and penalized least squares estimators that take into account a penalized least squares minimization problem. The article proceeds by discussing the main asymptotic properties separating results on mean square prediction error and results on L2 estimation error. It also describes some related models, including generalized functional linear models and FLR on quantiles, and concludes with a complementary bibliography and some open problems.


Author(s):  
Sreenivasa Charan Archakam ◽  
Keerthisikha Palur ◽  
Praveen Kumar Arava

The present study aimed to develop simple, accurate and precise FTIR and UV spectrophotometric methods for the quantification of Atenolol and Hydrochlorothiazide in bulk and tablet dosage forms. FT-IR method like classical least squares (CLS) was developed within the range of 2366.69-3433.44; 1564.40-1673.30 cm- UV methods like Cramer’s matrix method (method-I) and linear regression analysis (Method II) were developed and they are based upon constructing the matrix set by using molar absorptivity values at 275.60 nm and 270.40 nm. The assay values for FTIR- CLS method were 102% and 108 % for Atenololand Hydrochlorothiazide respectively. Cramer’s matrix method results were found to be 95.15% and 104% for Atenolol and Hydrochlorothiazide respectively and for linear regression method they were found to be 98.50% and 106% (w/w).


2006 ◽  
Vol 71 (11) ◽  
pp. 1207-1218
Author(s):  
Dondeti Satyanarayana ◽  
Kamarajan Kannan ◽  
Rajappan Manavalan

Simultaneous estimation of all drug components in a multicomponent analgesic dosage form with artificial neural networks calibration models using UV spectrophotometry is reported as a simple alternative to using separate models for each component. A novel approach for calibration using a compound spectral dataset derived from three spectra of each component is described. The spectra of mefenamic acid and paracetamol were recorded as several concentrations within their linear range and used to compute a calibration mixture between the wavelengths 220 to 340 nm. Neural networks trained by a Levenberg-Marquardt algorithm were used for building and optimizing the calibration models using MATALAB? Neural Network Toolbox and were compared with the principal component regression model. The calibration models were thoroughly evaluated at several concentration levels using 104 spectra obtained for 52 synthetic binary mixtures prepared using orthogonal designs. The optimized model showed sufficient robustness even when the calibration sets were constructed from a different set of pure spectra of the components. The simultaneous prediction of both components by a single neural network with the suggested calibration approach was successful. The model could accurately estimate the drugs, with satisfactory precision and accuracy, in tablet dosage with no interference from excipients as indicated by the results of a recovery study.


INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (03) ◽  
pp. 37-46
Author(s):  
Sapna M Rathod ◽  
Paresh U Patel

Four chemometric methods, namely Classical Least Square (CLS), Inverse Least Square (ILS), Partial Least Square (PLS) and Principal Component Regression (PCR), were developed for the simultaneous estimation of sofosbuvir and daclatasvir dihydrochloride in tablet formulation. Full factorial design was used to construct calibration set as well as validation set. Twenty five mixed solutions were prepared for calibration set and sixteen mixed solution of drugs were prepared for validation set. The absorbance of all prepared solutions was measured in the range of 230 nm to 335 nm at 16 wavelength points at an interval of 7 nm. Linearity was observed in the range of 10 – 90 µg/mL for sofosbuvir and 4 - 20 µg/mL for daclatasvir dihydrochloride. The developed chemometric methods were validated in terms of precision and accuracy as per ICH guidelines. The developed methods can be applied for the routine quantitative analysis of formulation.


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.


2021 ◽  
Vol 8 ◽  
Author(s):  
Yaoling Wang ◽  
Ruiyun Wang ◽  
Lijuan Bai ◽  
Yun Liu ◽  
Lihua Liu ◽  
...  

Background: Arterial stiffness was the pathological basis and risk factor of cardiovascular diseases, with chronic inflammation as the core characteristic. We aimed to analyze the association between the arterial stiffness measured by cardio-ankle vascular index (CAVI) and indicators reflecting the inflammation degree, such as count of leukocyte subtypes, platelet, and monocyte-to-lymphocyte ratio (MLR), etc.Methods: The data of inpatients from November 2018 to November 2019 and from December 2019 to September 2020 were continuously collected as the training set (1,089 cases) and the validation set (700 cases), respectively. A retrospective analysis of gender subgroups was performed in the training set. The association between inflammatory indicators and CAVI or arterial stiffness by simple linear regression, multiple linear regression, and logistic regression was analyzed. The effectiveness of the inflammation indicators and the CAVI decision models to identify arterial stiffness by receiver operating curve (ROC) in the training and validation set was evaluated.Results: The effect weights of MLR affecting the CAVI were 12.87% in men. MLR was the highest risk factor for arterial stiffness, with the odds ratio (95% confidence interval) of 8.95 (5.04–184.79) in men after adjusting the covariates. A cutpoint MLR of 0.19 had 70% accuracy for identifying arterial stiffness in all participants. The areas under the ROC curve of the CAVI decision models for arterial stiffness were >0.80 in the training set and validation set.Conclusions: The MLR might be a high-risk factor for arterial stiffness and could be considered as a potential indicator to predict arterial stiffness.


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