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![Figure1: Chemical structure of (a) Metformin hydrochloride, [b] Pioglitazone hydrochloride and (c) Melamine](profile/Amal-Khorshid/publication/327568165/figure/fig1/AS:682312928854016@1539687487005/Figure1-Chemical-structure-of-a-Metformin-hydrochloride-b-Pioglitazone.png)
Figure1: Chemical structure of (a) Metformin hydrochloride, [b] Pioglitazone hydrochloride and (c) Melamine
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![Figure1: Chemical structure of (a) Metformin hydrochloride, [b]...](profile/Amal-Khorshid/publication/327568165/figure/fig1/AS:682312928854016@1539687487005/Figure1-Chemical-structure-of-a-Metformin-hydrochloride-b-Pioglitazone_Q320.jpg)
simultaneous determination of Metformin hydrochloride and Pioglitazone hydrochloride in presence of Metformin impurity Melamine , both in bulk powder and in pharmaceutical preparation using spectrophotometric methods and thin layer chromatography . Method A used zero order spectrophotometric technique for determination of Pioglitazone at 268nm and...
Citations
... There are no clinically significant medication interactions between the studied drugs EMG, PGT, and RSV [2,8,15]; hence, there is no need for dose-adjustment while taking them together. There are several techniques for determining EMG, PGT, and RSV on an individual basis such as high-performance liquid chromatography (HPLC) [16][17][18][19][20][21][22], high-performance thin-layer chromatography (HPTLC) [23][24][25], ultra-performance liquid chromatography (UPLC) [26][27][28], liquid chromatography-tandem mass spectrometry (LC-MS/MS) [29][30][31][32], spectrophotometry [33][34][35], spectrofluorometry [36][37][38][39], and capillary electrophoresis [40,41]. A survey of the literature found that there is still no known technique for the simultaneous estimation of EMG, PGT, and RSV. ...
A simple, accurate, green and selective high-performance thin-layer chromatography (HPTLC) method has been developed and validated for the simultaneous estimation of empagliflozin, pioglitazone, and rosuvastatin in their synthetic ternary mixture and different biological fluids. These three drugs are used for the treatment of type 2 diabetes mellitus and dyslipidemia and have shown synergistic effects on cardiovascular outcomes. The ternary combination was separated on silica gel TLC plates G60 F 254 , utilizing a mixture of n -hexane‒ethyl acetate‒methanol‒glacial acetic acid in ratio (4.2:4:1.75:0.05, V/V ) as a developing system using ultraviolet (UV) detection at 230 nm. All experimental parameters were optimized with a linearity range of 5‒250 ng per band for each drug, with good sensitivity and low limit of detection values reached, namely 1.72, 1.79, and 1.52 ng per band for empagliflozin, pioglitazone, and rosuvastatin, respectively. The developed method was applied for separation of the studied drugs in their synthetic ternary mixture and different biological fluids, with good recovery results ensuring high efficiency of the proposed approach. Eco scale, green analytical procedure index, and AGREE metric tools were used to evaluate the greenness of the proposed method.
... For instance, there are many data analysis methods in the ML field that can perform the analysis of overlapped peaks in coupled reaction curves, such as the Fast Fourier Transform, 85 multivariate calibration methods, partial least squares regression, 86 and principal component regression. 87 Zhao et al. 88 utilized a linear regression model in ML to realize coupled detection of multiple substances, as shown in Fig. 5(b). The data were obtained by cyclic voltammetry in electrochemistry and then decoupled by linear regression model to obtain the prediction results of each component. ...
Electrochemical Immunosensing (EI) combines electrochemical analysis and immunology principles and is characterized by its simplicity, rapid detection, high sensitivity, and specificity. EI has become an important approach in various fields, such as clinical diagnosis, disease prevention and treatment, environmental monitoring, and food safety. However, EI multi-component detection still faces two major bottlenecks: first, the lack of cost-effective and portable detection platforms; second, the difficulty in eliminating batch differences and accurately decoupling signals from multiple analytes. With the gradual maturation of biochip technology, high-throughput analysis and portable detection utilizing the advantages of miniaturized chips, high sensitivity, and low cost have become possible. Meanwhile, Artificial Intelligence (AI) enables accurate decoupling of signals and enhances the sensitivity and specificity of multi-component detection. We believe that by evaluating and analyzing the characteristics, benefits, and linkages of EI, biochip, and AI technologies, we may considerably accelerate the development of EI multi-component detection. Therefore, we propose three specific prospects: first, AI can enhance and optimize the performance of the EI biochips, addressing the issue of multi-component detection for portable platforms. Second, the AI-enhanced EI biochips can be widely applied in home care, medical healthcare, and other areas. Third, the cross-fusion and innovation of EI, biochip, and AI technologies will effectively solve key bottlenecks in biochip detection, promoting interdisciplinary development. However, challenges may arise from AI algorithms that are difficult to explain and limited data access. Nevertheless, we believe that with technological advances and further research, there will be more methods and technologies to overcome these challenges.
... A literature survey revealed that various methods were reported for determination of MET alone by spectrophotometric methods (7,(13)(14)(15) or in the presence of its two potential impurities CN and MEL by chromatographic methods (9,(16)(17)(18). MET also was determined in the presence of CN by capillary zone electrophoresis (19) or in the presence of melamine and other drugs by chromatographic methods (20,21). ...
Background
The presented quadruple divisor spectrophotometric method was able to resolve and analyze a complex quintuple drug matrix with severe overlapped spectra without previous separation or extraction steps or need of complicated apparatus like chromatographic methods and had the advantage of being green as the solvent used was water.
Method
Simple, sensitive and precise quadruple devisor spectrophotometric method was developed for simultaneous determination of metformin, glipizide, and sitagliptin in presence of metformin potential impurities melamine and cyanoguanidine. The proposed method was applied for analysis of metformin, glipizide, and sitagliptin in pure form and pharmaceutical formulation (tablets). The developed method was validated and met the requirements for ICH guidelines with respect to linearity, accuracy, precision, specificity and robustness.
Results
A linear response was observed in the range of 2-27, 2-20, 1-20, 0.5-10, and 1-10 μg/mL for metformin, glipizide, sitagliptin, melamine and cyanoguanidine, respectively with a correlation coefficient of 0.9996 and 0.9998, 0.9997, 0.9997 and 0.9996 for metformin, glipizide, sitagliptin, melamine and cyanoguanidine, respectively.
Conclusion
The validated method was successfully applied for determination of the studied drugs in Janumet® and Engilor® tablets; moreover the results were statistically compared to those obtained by the reported RP-HPLC method and no significant difference was found between them; indicating the ability of proposed method to be used for routine quality control analysis of these drugs.
The instrumental analytical methods that have been developed and utilized for the determination of thiazolidinedione in bulk medications, formulations and biological fluids have been reviewed after an in-depth analysis of the literature published in a variety of analytical and pharmaceutical chemistry-related journals. The approaches covered by this research, which covers the years 2001-2022, include complex methods for analysis, chromatographic techniques and spectrometric analytical procedures. The mobile phase, flow rate, sample matrix, wavelength and other factors identified in the literature were just a few of the parameters used to evaluate thiazolidinediones. The present review focuses on the published analytical techniques for thiazolidinedione analysis that have been previously identified in the literature. The specified outcomes followed extensive learning, and the most recent advances in analytical methods for the identification of pioglitazone, pioglitazone HCl, rosiglitazone, rosiglitazone maleate and lobeglitazone were reviewed. Additionally, this article briefly discusses features of analytical discovery on thiazolidinediones, which will enable readers to access all discoveries in one place with precise outcomes.
Accurate, sensitive and green HPTLC chromatographic method was proposed for simultaneous determination of metformin, glipizide and sitagliptin in the presence of metformin potential toxic impurities melamine and cyanoguanidine. The separation was completed on silica gel HPTLC F254 plates using a mixture of ethyl acetate: methanol: ammonia: formic acid (7: 2: 0.2: 0.2, by volume) as a developing system with UV scanning for the developed bands at 235 nm. The Rf values for metformin, glipizide, sitagliptin, melamine and cyanoguanidine were 0.17, 0.84, 0.67, 0.47 and 0.75, respectively. Linear responses were observed in the ranges of 0.2-3, 0.07-1.5, 1.5-5, 0.8-4 and 0.4-2 μg/band with correlation coefficients of 0.9999, 0.9998, 0.9997, 0.9996 and 0.9998 for metformin, glipizide, sitagliptin, melamine and cyanoguanidine, respectively. The proposed method was validated as per ICH criteria with respect to linearity, accuracy, precision, specificity and robustness. The validated method was successfully applied for determination of the studied drugs in Janumet® and Engilor® tablets; also, the results were statistically compared to those obtained by the reported spectrophotometric method and no significant difference was found between them. This method permitted the accurate simultaneous determination of the studied drugs, indicating its ability to be used for routine quality control assays of these drugs.
Canagliflozin is an oral hypoglycemic drug recently formulated in combination with a biguanide, metformin hydrochloride, for improving its hypoglycemic action. Canagliflozin has one reported major degradation product, also metformin hydrochloride has one reported major degradation product, cyanoguanidine, and has a potential toxic impurity, melamine, that is reported to cause crystalluria that causes chronic kidney inflammation and nephrolithiasis leading to a renal failure. As per International Conference of Harmonization guidelines; a drug degradation product is classified as a type of drug impurities. Toxicity profiles of canagliflozin and metformin major degradation products were studied where in silico data disclosed toxicity too; the development of a specific chromatographic thin layer chromatographic assay was a must for quantification of such toxic related components along with the drugs in laboratory‐prepared mixtures as a superior study. The proposed method was validated as per the International Conference of Harmonization and applied for the assay of Vokanamet tablets. The separation was achieved using acetone:ethyl acetate:acetic acid (8:2:0.2, by volume) as scanning eluted bands at 205 nm. For minimal environmental impact; greenness profile appraisal of the proposed assay was performed by three greenness assessment approaches; analytical Eco‐Scale, Green Analytical Procedure Index, and Greenness metric approaches.
Simple, accurate, and precise four spectrophotometric methods were developed and validated for simultaneous determination of glimepiride and pioglitazone hydrochloride in their pharmaceutical formulation. The first spectrophotometric method was the dual-wavelength which determined glimepiride at 219.0 and 228.0 nm and pioglitazone hydrochloride at 268.0 nm. The second one is the first derivative of ratio spectra (DD1) spectrophotometry in which the peak amplitudes were used at 238.0 nm and 268.0 nm for glimepiride and pioglitazone hydrochloride, respectively. The third method is ratio subtraction in which glimepiride was determined at 228.0 nm in the presence of pioglitazone hydrochloride which was determined by extended ratio subtraction at 268.0 nm. The fourth method was the ratio difference to determine glimepiride and pioglitazone hydrochloride. Beer’s law was confirmed in the concentration range 2.50–15.00 µg mL-1, and 10.00–50.00 µg mL-1 for glimepiride and pioglitazone respectively for the four methods. The proposed methods were used to determine both drugs in their pure powdered form with mean percentage recoveries of 99.91 ± 1.117% for glimepiride and 99.76 ± 0.911% for pioglitazone hydrochloride in method (A). In method (B), the mean percentage recoveries were 100.12 ± 0.89% for glimepiride and 100.02 ± 1.06% for pioglitazone hydrochloride. In method (C) glimepiride was 100.01 ± 0.592% and 99.85 ± 0.845% for pioglitazone hydrochloride by extended ratio subtraction. And finally, in method (D) the mean percentage recoveries were 100.66 ± 0.670% for glimepiride and 99.92 ± 0.988% for pioglitazone hydrochloride. The developed methods were successfully applied for the determination of glimepiride and pioglitazone hydrochloride in pure powder and dosage form. The suggested methods were also used to determine both compounds in laboratory-prepared mixtures. The accuracy, precision, and linearity ranges of the developed methods were determined. The results obtained were compared statistically with the official method, and there was no significant difference between the proposed methods and the official method for accuracy and precision.
Background
In some cases, lifestyle changes are not enough to keep type 2 diabetes under control, there are several medications that may help. Metformin can lower your blood sugar levels. Glimepiride, make more insulin. Empagliflozin, prevent the kidneys from reabsorbing sugar into the blood and sending it out in urine.
Methods
Mean centering, double divisor, ratio spectra-zero crossing, and successive derivative were applied for estimation of metformin, empagliflozin, and glimepiride respectively, in their prepared laboratory mixtures and in pharmaceutical tablets, without prior chemical separation. The absorption spectra of the mentioned drugs were recorded in the range of 200-400nm.
Results
These methods were linear over the concentration ranges of 1.0-10, 2.5-30, and 1.0-10 µgmL-1 of metformin, empagliflozin, and glimepiride respectively. Mean centering for metformin were measured at 234 and 248 nm, empagliflozin and glimepiride had amplitude values at 276 and 262 nm, respectively. The derivative of double divisor was measured at 234, 278, and 288 nm for metformin, empagliflozin and glimepiride, respectively. The ratio spectra-zero crossing was quantifying at the amplitude values of the analytical signal at 234 and 274 nm for metformin and empagliflozin, respectively, whereas glimepiride was determined at 242 and 286 nm. The successive ratio of metformin, empagliflozin, and glimepiride were determined at 284, 242, and 266 nm, respectively.
Conclusion
The methods are validated according to the ICH guidelines where accuracy, precision and repeatability are found to be within the acceptable limit. The methods were studied and optimized, upon the validation linearity, precision, accuracy, LOD, LOQ and selectivity were proved to be operative for analysis of the specified drugs in pharmaceutical dosage configuration. The statistical illustration was done between the suggested methods with the reported methods with consideration to accuracy and precision no significant difference was found by student’s t-test, F-test and one-way ANOVA.
