scholarly journals Resolution of Ternary Mixture of Aspirin, Atorvastatin, and Clopidogrel by Chemometric-Assisted UV Spectroscopic and Liquid Chromatography Methods

2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Mahmoud Mohamed Issa ◽  
R'afat Mahmoud Nejem ◽  
Alaa Abu Shanab ◽  
Raluca-Ioana Stefan-van Staden

Two chemometrics-assisted UV spectrophotometric methods were proposed for the resolution of ternary mixtures without any chemical pretreatment. The first method is based on modification of H-point standard addition method which permits simultaneous analysis of three species from a unique calibration set by making the simultaneous addition of the three analytes. Quotient between the spectra of aspirin, atorvastatin, and clopidogrel was obtained and the results showed that simultaneous determination of aspirin, atorvastatin, and clopidogrel can be obeyed in the linear range 2.5–20 μg mL−1 of aspirin, 2.5–17.5 μg mL−1 of atorvastatin, and 2.5–20 μg mL−1 of clopidogrel in ternary mixture. The second method is based on the combination of the first derivative spectra and Cramer's matrix rule. In the matrix calculation, clopidogrel has zero crossing point at 316.8 and 212 nm, while for atorvastatin the zero crossing point at 250 nm where the matrix is greatly simplified and easily solved. The linear concentration ranges were 2.5–20 μg mL−1 aspirin, 2.5–17.5 μg mL−1 atorvastatin and 2.5–20 μg mL−1 clopidogrel in ternary mixtures. The results proved that the simultaneous determination of aspirin, atorvastatin, and clopidogrel could be obeyed. Both methods were applied for capsules containing the three ingredients and results were in good concordance with alternative liquid chromatography.

2020 ◽  
Vol 2020 ◽  
pp. 1-16 ◽  
Author(s):  
Shilan A. Omer ◽  
Nabil A. Fakhre

Three simple precise and accurate spectrophotometric methods are developed for simultaneous determination of ternary mixtures of carboxin, chlorpyrifos, and tebuconazole residues in cabbage grown in the experimental field. The first method is a double divisor-ratio spectra derivative that relies on the derivative of ratio spectra and attained through dividing the absorption spectra of the ternary mixture by the sum of standard spectrum of a mixture of two from three components, using methanol as a solvent and measuring CAR at 242 nm, CHL at 236 nm, 276 nm, and 300 nm, and TEB at 226 nm. The second method is a successive derivative of ratio spectra which determined CAR at 256 nm and 258 nm, CHL at 290 nm and 292 nm, and TEB at 226 nm and 228 nm. The third method is a mean centering of ratio spectra where CAR, CHL, and TEB were measured at 306 nm, 280 nm, and 240 nm, respectively. These procedures do not involve any previous separation. The extraction of analytes was carried out by using acetonitrile, and the procedure of purification was fulfilled by dispersive solid-phase extraction with a primary-secondary amine (PSA). The proposed methods showed excellent linearity range for three spectrophotometric methods over the concentration ranges of 1–30 μg/mL, 1–50 μg/mL, and 1–45 μg/mL for carboxin, chlorpyrifos, and tebuconazole, respectively. The analytical characteristics such as detection limit, determination limit, relative standard deviation, and accuracy of the three methods were performed. The limits of detection were in the range of 0.153–0.260 μg/mL for carboxin, 0.137–0.272 μg/mL for chlorpyrifos, and 0.109–0.205 μg/mL for tebuconazole with limits of quantification lower than 0.790, 0.824, and 0.621 μg/mL for CAR, CHL, and TEB, respectively. The recoveries ranged from 87.02% to 94.53% for carboxin, 92.32% to 108.53% for chlorpyrifos, and 87.19% to 98.00% for tebuconazole with relative standard deviations less than 5.91%, 5.99%, and 5.53% in all instances for carboxin, chlorpyrifos, and tebuconazole, respectively. The results obtained from the proposed methods were compared statistically by using one-way ANOVA, and the results revealed that there were no significant differences between three different spectrophotometric methods. The suggested methods can be applied with great success to the simultaneous estimation of carboxin, chlorpyrifos, and tebuconazole residues in cabbage samples.


2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Shilan A. Omer ◽  
Nabil A. Fakhre

In this study, three simple and accurate spectrophotometric methods for simultaneous determination of pyriproxyfen and chlorothalonil residues in cucumbers and cabbages grown in experimental greenhouse were studied. The first method was based on the zero-crossing technique measurement for first and second derivative spectrophotometry. The second method was based on the first derivative of the ratio spectra. However, the third method was based on mean centering of ratio spectra. These procedures lack any previous separation steps. The calibration curves for three spectrophotometric methods are linear in the concentration range of 1–30 μg·mL−1 and 0.5–7 μg·mL−1 for pyriproxyfen and chlorothalonil successively. The recoveries ranged from 82.12–97.40% for pyriproxyfen and 81.51–97.04% for chlorothalonil with relative standard deviations less than 4.95% and 5.45% in all instances for pyriproxyfen and chlorothalonil, respectively. The results obtained from the proposed methods were compared statistically by using one-way ANOVA, and the results revealed there were no significant differences between ratio spectra and mean centering methods with the zero-crossing technique. The proposed methods are successfully applied for the simultaneous estimation of the residue of both pesticides in cucumber and cabbage samples.


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.


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.


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