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... Empagliflozin, 1-chloro-4-(glucopyranos-1-yl)-2-(4-(tetrahydrofuran-3-yloxybenzyl) benzene, [ Figure 1 (a)] is an orally available competitive inhibitor of Sodium-glucose Co-transporter-2 (SGLT2) with anti-hyperglycemic activity. Empagliflozin function by inhibiting SGLT-2 present in proximal tubules in the kidneys. ...
Context 2
... reduces renal reabsorption of glucose leads to increase in urinary excretion of glucose and act as a antidiabetic agent for treatment of type-2 diabetes. 1 Metformin [ Figure 1 (b)] is antihyperglycemic agent acts by inhibition of hepatic glucose output and therefore, the liver is most likely the principle site of Metformin function. 2 Chemically Metformin is 1-carbamimidamido-N,N-dimethylmethanimidamide. ...
Context 3
... calibration curve for MET and EN were observed as linear in the concentration range of 5000-30000 ng band -1 and 125-750 ng band -1 respectively with regression coefficient (r 2 ) values of 0.992 and 0.994 respectively ( Figure 10). The statistical data for linearity is summarized in Table 5. ...
Context 4
... chromatogram of possible H 2 O 2 degradation product appeared as additional peak bands at R f values 0.59, 0.65 (approximate 5.63%, 2.04 % degradation) along with the R f values of 0.50 and 0.82 for MET and EN respectively. (Figure 13) ...
Context 5
... chromatogram of possible wet degradation product appeared as additional peak bands at R f values 0.58, 0.62, 0.80 (approximate 3.45%, 2.34%, 1.23% degradation) along with the R f values of 0.50 and 0.82 for MET and EN respectively. (Figure 14) ...
Context 6
... chromatogram of possible wet degradation product appeared as additional peak bands at R f values at 0.55, 0.65 (about 4.92%, 3.14 % degradation) along with the R f values of 0.50 and 0.82 for MET and EN respectively. (Figure 15) ...
Context 7
... chromatogram of possible wet degradation product appeared as additional peak bands at R f values at 0.65 (about 1.20 % degradation) along with the R f values of 0.50 and 0.82 for MET and EN respectively. (Figure 16) ...
Context 8
... Empagliflozin, 1-chloro-4-(glucopyranos-1-yl)-2-(4-(tetrahydrofuran-3-yloxybenzyl) benzene, [ Figure 1 (a)] is an orally available competitive inhibitor of Sodium-glucose Co-transporter-2 (SGLT2) with anti-hyperglycemic activity. Empagliflozin function by inhibiting SGLT-2 present in proximal tubules in the kidneys. ...
Context 9
... reduces renal reabsorption of glucose leads to increase in urinary excretion of glucose and act as a antidiabetic agent for treatment of type-2 diabetes. 1 Metformin [ Figure 1 (b)] is antihyperglycemic agent acts by inhibition of hepatic glucose output and therefore, the liver is most likely the principle site of Metformin function. 2 Chemically Metformin is 1-carbamimidamido-N,N-dimethylmethanimidamide. ...
Context 10
... calibration curve for MET and EN were observed as linear in the concentration range of 5000-30000 ng band -1 and 125-750 ng band -1 respectively with regression coefficient (r 2 ) values of 0.992 and 0.994 respectively ( Figure 10). The statistical data for linearity is summarized in Table 5. ...
Context 11
... chromatogram of possible H 2 O 2 degradation product appeared as additional peak bands at R f values 0.59, 0.65 (approximate 5.63%, 2.04 % degradation) along with the R f values of 0.50 and 0.82 for MET and EN respectively. (Figure 13) ...
Context 12
... chromatogram of possible wet degradation product appeared as additional peak bands at R f values 0.58, 0.62, 0.80 (approximate 3.45%, 2.34%, 1.23% degradation) along with the R f values of 0.50 and 0.82 for MET and EN respectively. (Figure 14) ...
Context 13
... chromatogram of possible wet degradation product appeared as additional peak bands at R f values at 0.55, 0.65 (about 4.92%, 3.14 % degradation) along with the R f values of 0.50 and 0.82 for MET and EN respectively. (Figure 15) ...
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Citations
... The literature survey reveals that many UV, HPLC, and HPTLC methods have been reported for MFH alone [8][9][10][11] and in combination with other drugs. [12][13][14][15][16] For EGT, only one UV and one RP-HPLC method is reported for its estimation. 17,18 However, no method has been reported for the simultaneous determination of MFH and EGT in combination. ...
Evogliptin (EGT) is used in fixed-dose combination with metformin hydrochloride (MFH) for a better glycemic control in Type 2 diabetes mellitus. To date, no method is available for simultaneous estimation of these drugs. In the present study, an UV spectrophotometric method was developed in distilled water, an environment-friendly solvent using the simultaneous equation technique to simultaneously determine EGT and MFH in bulk and tablet dosage form. The developed method was validated and applied to commercial tablet dosage forms containing EGT and MFH in combination. With a great correlation value (R2>0.998), the analytes displayed good linearity in the range of 10-100 μg mL-1. The low percent relative standard deviation proved the methods' precision. The methods' accuracy was demonstrated by excellent recovery. Thus, the developed method was found to be simple, environment-friendly, fast, specific, precise, and accurate, and it may be effectively used for routine analysis of EGT and MFH in bulk and their combined tablet dosage form.
... Literature survey revealed that analytical methods have been reported for Empagliflozin and Atorvastatin either individually or in combination with other drugs. Analytical methods including UV spectrophotometry [13], [14], HPLC [15]- [20], LC-MS [21]- [27], and HPTLC [27][28][29][30][31][32] have been reported for the determination of Empagliflozin in pharmaceutical products and biological fluids. Atorvastatin is reported to be determined either alone or in combination with other drugs in pharmaceutical preparation and biological matrices by analytical methods involving UV spectrophotometry [33][34][35][36][37][38], HPLC [39][40][41][42][43][44][45][46], LC-MS [47][48][49][50][51], and HPTLC [52][53][54][55][56][57]. ...
Diabetes and cardiovascular disease are rising global health concerns and in around 85% of cases, patients are having both these diseases as a comorbid condition. Such patients administer drugs belonging to both antidiabetic and antihyperlipidemic class. Managing diabetes mellitus along with cardiovascular disease is done by controlling blood glucose level and cholesterol level by adapting antidiabetic and antihyperlipidemic drug therapy respectively with their simultaneous administration. Selection of the most accurate drugs and their effective dose regime is very important to avoid further severe complications. Empagliflozin is prescribed as a first-line drug for diabetes treatment and Atorvastatin is the preferred one in cardiovascular disease. The dual effect of Atorvastatin on the blood glucose level creates a need for monitoring of its concentration in patients consuming simultaneously an antidiabetic drug like Empagliflozin. The proposed method is an attempt to develop an HPTLC method for simultaneous estimation of Atorvastatin and Empagliflozin in human plasma. Chromatographic separation of drugs was performed over TLC plates pre-coated with silica gel 60F254 using toluene: ethyl acetate: methanol: formic acid (12:5:3:0.5 v/v/v/v) as the mobile phase via a linear ascending technique. Detection and quantification were carried out at a wavelength 235 nm. The method was validated according to the European Medicines Agency ICH guideline M10 on Bioanalytical Method Validation and gave satisfactory results. The developed method can be successfully employed for simultaneous estimation of Empagliflozin and Atorvastatin from human plasma of patients with the comorbid condition of diabetes and cardiovascular disease.
... In addition, REM helps in reducing the body weight and blood pressure in diabetes mellitus patients. [8][9][10] Many analytical methods were illustrated for the estimation of MET from pharmaceutical preparations and plasma by spectroscopic, 11,12 HPLC, [13][14][15] HPLTC, 16 LC-MS, 17,18 and CZE, 19,20 alone and with other drugs. Few analytical procedures were also depicted in the texts for the analysis of REM. ...
... Seven aliquots of MET and REM working standard solutions were transferred into 10 ml calibrated flasks, to obtain the amount of MET in the series of 2.5 to 30 µg/ ml (2.5, 5, 10, 15, 20, 25, 30) and REM in the range of 1 to 24 µg/ml (1,4,8,12,16,20, 24 µg/ml). UV absorption spectra were documented for these solutions in the range of 200 nm to 300 nm against dilute ethanol as solvent. ...
... Further, derivatization removes the effect of other analytes and formulation measuring only one analyte at zero-crossing wavelength of another analyte. In the present work, UV spectra of mixture of MET (2.5, 5, 10, 15, 20, 25 and 30 µg/ml) and REM (1,4,8,12,16,20 and 24 µg/ml) was divided with spectrum of REM (20 µg/ml) for measurement of MET. Different concentration spectra of REM were tried, however, 20 µg/ml showed better recovery. ...
The result of pharmaceutical industry research for the new class and the new combination of drugs for the treatments of diabetes is the newly approved combination of metformin (MET) and remogliflozin (REM). For the quality control of this formulation, three smart, reproducible and non-sophisticated spectroscopic techniques were developed by modification of UV spectra. The first two methods were based on the measurements of the peak height of the third derivative and second derivative ratio spectra of MET and REM and the third method was the constant center spectrum subtraction method. The proposed methods exhibited Beer’s law in the range of 2.5 to 30 μg/ml and 1 to 24 μg/ml for MET and REM correspondingly by all three methods. The mean percentage recovery was found to be in the range of 99.08% to 100.15% for MET and 98.73% to 100.27% for REM. Further, both analytes were quantified from the formulation using proposed spectroscopic methods with high accuracy. Comparison of all three methods with the reported HPLC method showed no variation in the assay outcomes in relation to accuracy and precision. The suggested techniques are simple, accurate and reproducible, hence could be used for regular quality control of formulation consisting of MET and REM.
... Several methods are illustrated in the literature for the analysis of metformin alone and along with different classes of agents from formulations and body fluids. Recent methods reported were UV-spectrophotometry [19][20][21], RP-HPLC [22][23][24][25], HPTLC [24,25], capillary electrophoresis [26,27] and LCMS [28][29][30][31][32]. There were few reports in the literature for the simultaneous estimation of metformin along with SGLT-2 inhibitors [32,33]. ...
... Several methods are illustrated in the literature for the analysis of metformin alone and along with different classes of agents from formulations and body fluids. Recent methods reported were UV-spectrophotometry [19][20][21], RP-HPLC [22][23][24][25], HPTLC [24,25], capillary electrophoresis [26,27] and LCMS [28][29][30][31][32]. There were few reports in the literature for the simultaneous estimation of metformin along with SGLT-2 inhibitors [32,33]. ...
The recent trend in green analytical chemistry is the development of green analytical methods using environmentally friendly solvents. Therefore, three ecofriendly manipulated UV spectroscopic techniques have been validated for the concurrent quantification of newly approved remogliflozin etabonate (REM) and metformin HCl (MET) tablets using water as a solvent. The first method was established using first derivative absorption spectroscopic method by determining the peak amplitude at 233.0 nm for REM and 252.2 nm for MET, a zero crossing of one the component. The second and third methods were based on the peak amplitude difference and first-order derivative absorption of the ratio spectra developed by the manipulation of scanned UV spectra. REM and MET showed good linearity in the series of 1–20 µg ml−1 and 2.5–35 µg ml−1, respectively, by all three methods with an excellent correlation coefficient (r2 ≥ 0.998). Further, the proposed UV spectroscopic techniques were validated as per International Council for Harmonization guidelines. The methods showed good sensitivity, accuracy, and precision. Anticipated procedures were effectively utilized for the concurrent quantification of REM and MET in laboratory prepared mixtures and tablets. The high percent recovery with low standard deviation found for both analytes by all three methods confirms the accuracy and precision of the procedures. Finally, the greenness of the proposed spectroscopic methods, evaluated by semi-quantitative and quantitative methods, showed the eco-friendly nature of the methods. Furthermore, the proposed approaches were simple, accurate, sensitive, economic, and environmentally friendly and hence can be utilized for regular quality control of REM and MET formulation.
The newly developed stability‐indicating RP-HPLC method is simple, robust and validated on the basis of ICH guidelines for the simultaneous determination of Empaglifozin and Metformin hydrochloride in the tablet. Retention times under the optimized condition were 2.104 and 4.0822min for Metformin and Empaglifozin respectively. This research article indicates best separation of Empaglifozin and Metformin from their degradation products. Separation was achieved on a Sunniest ECO C18, 250mm x 4.6mm, 5µm analytical column at wavelength of 225nm, using a mobile buffer (pH-1.8): acetonitrile (50:50) in an isocratic elution mode at a flow rate of 1.2ml/min, Injection volume: 10µl and run time 6mins. The %RSDs for the precision studies was less than 1.5% for both drugs. The %RSD was less than 1.5% in all the parameters of robustness. The forced degradation studies were carried by using 0.1N HCl, 0.1 N NaOH and % 3 H2O2 and there is only % 7.2 degradation in an acidic medium for emplaglifozin and 11.63% for Meformin where as there was nothing degradation in basic and oxidative method. The analyte peaks were clearly separated from the degradant peaks in forced degradation studies. So this method is a fast, sensitive, robust and efficient high performance liquid chromatographic method for the concurrent determination of Metformin and Empaglifozin in their combination, and thus this method can be effectively employed for routine quality control works.
Molecular modeling is the science of representing molecular structures numerically and simulating their behavior with the equations of quantum and classical physics. Coupling molecular modeling and simulation with chromatographic resolution for pharmaceutical products constitutes a new technique in pharmaceutical analysis. An innovative high-performance liquid chromatographic (HPLC) methodology was developed for the quantification of metformin hydrochloride (MET), empagliflozin (EMP), and canagliflozin (CAN) in bulk, laboratory-developed combinations, pharmaceutical tablets, and in the presence of melamine. Chromatographic separation was accomplished using a Symmetry column with 0.03 M potassium dihydrogen phosphate buffer and 0.02 M heptane sulphonic acid: acetonitrile as the mobile phase. Molecular modeling using molecular operating environment software was applied to properly select the stationary phase suitable for the developed HPLC method. Additionally, molecular modeling estimates and validates binding between the studied analytes and the stationary phase to clarify and explain the chromatographic separation and elution order. In accordance with the International Conference of Harmonization recommendations, the method was validated in terms of linearity, accuracy, precision, and selectivity. The linearity ranges (μg/ml) were 200-1500 (MET), 2-15 (EMP), and 20-150 (CAN) and the limit of detection values were in the ranges of 0.17-54.58 μg/ml. Analysis of pharmaceutical tablets using the suggested approach yielded satisfactory outcomes. As a result, it might be used in quality control laboratories to analyze the aforementioned medications.
For the purpose of analyzing empagliflozin, a stability indicating high performance thin layer chromatographic method was developed. This method was optimized using design of experiment. In order to optimize the process, independent variables such as the proportion of isopropyl alcohol in the mobile phase, the duration of time that the chamber was saturated and the distance of mobile phase travelled were considered. On an aluminum plate that had previously been coated with silica gel, development was carried out with the assistance of twin trough glass chambers in ascending lines. The findings from these studies led to the selection of a mobile phase that had a composition of ammonium acetate (2 %), triethylamine and isopropyl alcohol in the ratio of 4:1:5 (V/V/V), and this mobile phase was utilized in the process of method development using central composite design approach. The saturation time was established at 10 minutes, and the ultraviolet detection was performed at a wavelength of 237 nm. The value 0.82 was discovered to be the retention factor (Rf ) for empagliflozin. The method was linear, precise and accurate over the entire concentration range examined (100-600 ng band-1), along with correlation coefficient value of 0.992. The proposed method is quick and selective, and a straightforward method of sample preparation and analysis for empagliflozin in its bulk and commercially available dosage forms. The stability of the drug was tested under a variety of different stress conditions in accordance with ICH guidelines, and the results obtained from the force degradations indicate that the developed method is appropriate for stability studies.
Pharmaceutical analysis is necessary at all stages of the drug development process, including formulation development, stability studies, and quality control. It is also used for characterizing the composition of different dosage forms in quantitative and qualitative ways. Comprehensive literature survey forms the foundation stone for the focused analysis of research activity. This review article represents the collection and discussion of various analytical methods available in the literature for the determination of oral anti-diabetic drugs like Empagliflozin (EMPA), Linagliptin (LINA) and Metformin hydrochloride (MET) for the treatment of type II diabetes mellitus, consisting of UV, TLC, HPTLC, and HPLC. The anticipated review provides details about the comparative utilization of various analytical techniques for the determination of EMPA, LINA and MET. This review article can be effectively explored to conduct future analytical investigation for the estimation of selected drugs in pharmaceutical and biological samples.
Background
Fixed-dose combinations (FDCs) are renowned formulations that contain two or more drugs pooled in a single dosage form. Their recognition is justified due to several advantages, such as impending therapeutic efficacy, reducing the episodes of adverse drug effects, having pharmacokinetic advantages, reducing pill burden, reducing the dose of individual drugs, and decreasing drug resistance development.
Objective
Recently, an FDC tablet of remogliflozin etabonate (100 mg), vildagliptin (50 mg), and metformin HCl (500/1000 mg) has been approved for the treatment of type 2 diabetes mellitus. No analytical method has been reported thus far for this newly approved combination.
Methods
Thus, this review collected and simplified information on reported analytical techniques and physicochemical and biological properties for the above-cited FDCs. The authors have explored various authenticated scientific journals, and simplified information was presented to meet the objectives.
Results
The reported methods are spectroscopy (40%, 20% & 33%), HPTLC (10%, 14% & 20%), HPLC (50%, 49% & 41%), hyphenated techniques (Nil, 14% & 5%) and electrophoresis methods (Nil, 2% & 1%) for remogliflozin etabonate, vildagliptin and metformin HCl, respectively.
Conclusion
Such extensive data would be useful to analysts in developing an analytical method for the analysis of the recently approved FDCs
