Abstract
The UPLC methodology was used to establish a method for determining the qualitative and quantitative content of teneligliptin and remogliflozin tablets in oral solid dose form, as no simultaneous method was available. The developed liquid chromatography method consists of an X-Bridge C18 100 mm × 3.5 mm, 2.1 mm column with an economical 0.2 mL/min flow rate. A wavelength of 248 nm was used for detection, and the temperature of the column compartment was 30 °C. The method was evaluated using a static tool quality by design after it was validated as per the regulations. The data from validation result in linearity for both analytes with a correlation coefficient of more than 0.999. The accuracy data were found from a minimum of 98.1 to a maximum of 100.9. All of the validation results met the acceptance criteria. The stability of the analytical solutions proved for 24 h at bench and refrigerator temperatures. Studies of force degradation proved the stability indicating the nature of the method. A factorial design was used to evaluate the method performance.
1. Introduction
Remogliflozin etabonate is a sodium glucose cotransporter 2 inhibitor, a treatment with verbal antidiabetics. Remogliflozin etabonate reduces the amount of excess sugar that you get from your body through the urine. Remogliflozin etabonate lowers the amount of glucose in the blood. Remogliflozin etabonate works by controlling blood sugar levels and helping to lower blood sugar levels. The chemical formula for remogliflozin etabonate is C26H38N2O9, and the molecular weight is 522.595.
Teneligliptin is an antidiabetic dipeptidyl peptidase-4 (DPP-4) inhibitor. The sum of insults delivered by the pancreas can be expanded by teneligliptin. The hormones that increase blood sugar levels are reduced by teneligliptin. The amount of sugar in the blood is controlled by teneligliptin. Zita plus R tablet can be used to control blood sugar levels. The chemical formula for teneligliptin is C22H30N6OSe, and the molecular weight is 426.58. The structures of both analytes are shown in Figure 1.
Figure 1.
Chemical structure of remogliflozin and teneligliptin.
Remogliflozin etabonate and teneligliptin combination phrasings are available in oral solid dosage form. The quantification of both analytes in the formulation is the quality, safety, and efficacy factor of the dosage form. The quantification method is needed to identify the content present in the formulation. The current research targeted the content determination for the targeted formulation. There was only one article available for the content determination using the UV spectroscopy,1 but this method is not suitable for shelf life analysis due to the lack of stability indicating nature. Attimarad et al. developed simultaneous quantification of two binary formulations containing remogliflozin and gliptins.2 Dhara et al. developed a UV spectroscopic method for determination of remogliflozin etabonate in bulk and tablet dosage form.3 Attimarad et al. developed multicomponent antidiabetic formulation analysis.4 Shah et al. developed a liquid chromatographic method for the estimation of remogliflozin etabonate.5 Itigimatha et al. developed remogliflozin etabonate in pure and pharmaceutical formulations analysis.6 Attimarad et al. developed multicomponent antidiabetic formulation by the HILIC method.7 Vinodbhai developed the estimation of remogliflozin and vildagliptin in pharmaceutical dosage form method.8 Ali et al. developed quantification of vildagliptin and remogliflozin etabonate in bulk drug and formulations method.9 Jaiswal et al. developed the estimation of metformin hydrochloride and remogliflozin enabonate in pharmaceutical dosage form method.10 Kumar et al. developed teneligliptin by the RP-HPLC method.11 Kant et al. developed metformin, gliclazide, pioglitazone, dapagliflozin, empagliflozin, saxagliptin, linagliptin, and teneligliptin using the central composite design method.12 Lokhande developed teneligliptin by using the RP-HPLC method.13 Biswas et al. developed teneligliptin in tablet dosage form by the RP-HPLC method.14 Bichala et al. developed estimation of metformin and teneligliptin in its bulk and tablet dosage form by using the RP-HPLC method.15 Musmade et al. developed the impurity profiling method and validation of metformin hydrochloride and teneligliptin hydrobromide hydrate in their combination tablet dosage form by using the RP-HPLC method.16 Shah et al. developed estimation of antidiabetic drug teneligliptin by the HPTLC method.17 Kumar et al. developed teneligliptin by the RP-HPLC method.18 These available research targeted individual determination and combination with some other formulations. The detailed literature revealed that no single determination method was available, and only individual content determination methods are available for both analytes. The present research work aimed to create a simple, sensitive, and environmentally friendly content determination method for the combination dosage form. Quality by design is a stationary tool, which is useful for optimizing the method and assessing the system performance with minimum changes.19,20 The presently developed method originally optimized conditions and estimated the system performance with the factorial design by studying the critical method parameters with design expert software.21
2. Materials and Methods
2.1. Chemicals, Reagents and Materials
The standard gift sample of remogliflozin etabonate and teneligliptin tablets and placebo was from a reputed pharma company. Standards are procured from the international supplier. Milli Q water available from the Millipore purification system was used. Analytical grade was used for hydrochloric acid, whereas HPLC grade was used for acetonitrile, triethylamine, orthophosphoric acid, and methanol.
2.2. Instruments and Software
The ACQUITY TUV UPLC has a photodiode array detector that was used for the entire research. The research was carried out using Empower software. The Skymen Ultrasonicator and HA vacuum pump were used for buffer and mobile phase degassing. Using a Mettler-Toledo Pan Balance (Model ME2002TE/02), a Mettler-Toledo Semi-Micro Balance (Model XPE105DR), and a Sartorius Microbalance (Model MSXLSGEA1), standards and samples were weighed. The Yesi drug photo stability chamber was subjected to forced degradation investigations. The column from Waters was used for the separation. The DoE trials in the method evaluation were carried out using Stat-ease Inc., Minneapolis, USA’s Design Expert software version 13.
2.3. Analytical Solution Preparation
2.3.1. Standard Solution Preparation
Fifty mg of remogliflozin and 5 mg of teneligliptin standards were accurately weighed and transferred into 100 mL clean dry volumetric flasks; 10 mL of diluent was added; it was then sonicated for 10 min and made up to the final volume with diluent (500 μg/mL teneligliptin and 50 μg/mL of remogliflozin). One mL of the two stock solutions was taken into a 10 mL volumetric flask and made up to 10 mL with diluent (50 μg/mL remogliflozin and 5 μg/mL of teneligliptin).
2.3.2. Preparation of Sample Stock Solutions
Ten tablets were weighed and ground into fine powder, and an equivalent to 1 tablet was weighed and transferred to a 100 mL volumetric flask; to this, 50 mL of diluent was added and sonicated. The volume was made up to 50 mL with diluent and filtered through 0.45 μm or finer porosity membrane filter (1000 μg/mL remogliflozin and 100 μg/mL of teneligliptin). A 0.5 mL portion of filtered sample stock solution was transferred to a 10 mL volumetric flask and made up with diluent (50 μg/mL remogliflozin and 5 μg/mL of teneligliptin).
2.4. Forced Degradation Study
The safety and efficacy of drug products are dependent on the chemical stability of the molecule. Stability data is required by the FDA and ICH to understand the quality of the drug product.22−26 To find the stability of the drug product as well as to see whether the drug product forms any new impurities in the stability that impact the quantitative analysis and efficacy of the drug product, the drug product was subjected to forced degradation studies. A forced degradation study was performed on the drug product and placebo to see whether there was interference with the analyte. Acid, alkali, oxidizer, thermal, neutralization, and photostability studies were performed.
2.4.1. Acid Degradation Studies
Ten tablets were weighed and ground into fine powder, and an equivalent to 1 tablet is weighed and transferred to 100 mL volumetric flask; to this, 50 mL of diluent was added and sonicated. Volume was made up to 50 mL with diluent and filtered through 0.45 μm or finer porosity membrane filter (1000 μg/mL remogliflozin and 100 μg/mL of teneligliptin). To 1 mL of stock solution remogliflozin and teneligliptin, 1 mL of 2 N hydrochloric acid was added and refluxed for 30 min at 60 °C. For UPLC study, the resultant solution was diluted to obtain 50 and 5 ppm solutions, 10 μL was injected into the system, and the chromatograms were recorded to assess the stability of the sample.
2.4.2. Alkali Degradation Studies
Ten tablets were weighed and ground into fine powder, and an equivalent to 1 tablet is weighed and transferred to 100 mL volumetric flask; to this, 50 mL of diluent was added and sonicated. The volume was made up to 50 mL with diluent and filtered through 0.45 μm or finer porosity membrane filter (1000 μg/mL remogliflozin and 100 μg/mL of teneligliptin). To 1 mL of stock solution remogliflozin and teneligliptin, 1 mL of 2 N sodium hydroxide was added and refluxed for 30 min at 60 °C. For UPLC study, the resultant solution was diluted to obtain 50 and 5 ppm solutions, 10 μL was injected into the system, and the chromatograms were recorded to assess the stability of the sample.
2.4.3. Oxidation Degradation Studies
Ten tablets were weighed and ground into fine powder, and an equivalent to 1 tablet is weighed and transferred to 100 mL volumetric flask; to this, 50 mL of diluent was added and sonicated. The volume was made up to 50 mL with diluent and filtered through 0.45 μm or finer porosity membrane filter (1000 μg/mL remogliflozin and 100 μg/mL of teneligliptin). To 1 mL of stock solution of remogliflozin and teneligliptin was added 1 mL of 20% hydrogen peroxide (H2O2) separately. The solutions were kept for 30 min at 60 °C. For the UPLC study, the resultant solution was diluted to obtain 50 and 5 ppm solutions, 10 μL was injected into the system, and the chromatograms were recorded to assess the stability of the sample.
2.4.4. Thermal Degradation Studies
The standard drug solution was placed in an oven at 105 °C for 6h to study dry heat degradation. For the UPLC study, the resultant solution was diluted to obtain 50 and 5 ppm solutions, 10 μL was injected into the system, and the chromatograms were recorded to assess the stability of the samples.
2.4.5. Photostability studies
The photochemical stability of the drug was also studied by exposing the 500 and 50 ppm solutions to UV Light by keeping the beaker in a UV chamber for 7 days or a 200 W h/min photostability chamber. For the UPLC study, the resultant solution was diluted to obtain 50 and 5 ppm solutions, 10 μL was injected into the system, and the chromatograms were recorded to assess the stability of the sample.
2.4.6. Neutral Degradation Studies
Stress testing under neutral conditions was studied by refluxing the drug in water for 6 h at a temperature of 60 °C. For UPLC study, the resultant solution was diluted to obtain 20 and 80 ppm solutions, 10 μL was injected into the system, and the chromatograms were recorded to assess the stability of the sample.
2.5. Chromatography Conditions
The qualitative and quantitative methods were developed by using the Waters X-Bridge C18 100 mm × 3.5 mm, 2.1 μm column. The mobile phase consists of 35:65 v/v buffer (0.1% Orthophosphoric acid buffer): Methanol. The flow rate for the separation was 0.2 mL/min, and the volume of the injection was 10 μL. The temperature of the column chamber was 30 °C, and the detection took place at 248 nm. The overall run time was only 3.0 min. Based on the solubility of the drugs, diluent was selected which was methanol and water taken in the ratio of 65:35 and sonicated for 15 min and Filter with 0.45 μm nylon filter.
3. Results and Discussion
3.1. Optimization of chromatography method
The purpose of this research is to develop and validate a precise, accurate, linear, robust, and stability-indicating chromatographic method to determine both analytes remogliflozin etabonate and teneligliptin in solid oral dosage formulation in UPLC. UPLC techniques were used for development in light of green chemistry and economy due to the fast elution. Predicated on the physicochemical properties of both analytes, a reverse-phase Waters X-Bridge C18 100 mm × 3.5 mm, 2.1 mm column was selected for initial optimization. Water, acetonitrile, and methanol were used for cumulation mobile phases selected for initial chromatography conditions with a 0.3 mL/min flow rate; the column compartment temperature was chosen at 30 °C to maintain the stable condition. Both standard solutions were injected in the initial chromatography conditions, and the UV spectra were recorded to identify the wavelength for quantification. 248 nm was selected for further studies; both peaks were eluted at void volumes; and the peak was eluted with fronting and tailings. Elution denotes that water as a buffer does not work for the elution of both analytes; buffer strength was needed for better chromatography. To increment the buffer strength, 0.1% OPA (Ortho phosphoric acid) and 0.1% TFA (trifluoroacetic acid) buffers are chosen, and the trials were performed with different ratios of mobile phase with methanol. Methanol was selected because it was economically cheaper than the acetonitrile. 0.1% OPA buffer providing symmetrical peak shapes compared with the 0.1% TFA and 0.1% OPA is selected as the buffer of final optimization. Different ratios of mobile phase were endeavored with 0.1% buffer and methanol with a flow rate of 0.2 mL/min for slow elution. Conclusively, the combination of buffer and methanol in the ratio 35:65 v/v with a Waters X-Bridge C18 100 mm × 3.5 mm, 2.1 mm column was found suitable for the current research. The obtained chromatogram showed that the remogliflozin etabonate was eluted at a retention time of about 1.3 min, and teneligliptin was eluted at a retention time of about 1.6 min. The final chromatogram shown in Figure 2.
Figure 2.
Standard solution chromatogram in the significant trials and in the final optimized condition.
3.2. Method Validation Study
3.2.1. Specificity
To determine the specificity of the method, injections of standard solution, diluent, placebo, and sample were used. The resulting sample solutions were tested for the retention time and maximum purity. The elution times of the placebo peaks and degradants were recorded. The placebo or diluent did not interfere with the analytes. Results are mentioned in Table 1.
Table 1. System Suitability, Linearity, Accuracy, and Precision Results for Remogliflozin and Teneligliptin.
| parameters | remogliflozin | teneligliptin |
|---|---|---|
| system suitability | ||
| USP tailing factor | 1.13 | 1.07 |
| USP plate count (N) | 5924 | 8430 |
| resolution | 1.55 | 4.20 |
| Rt (min) | 1.352 | 1.649 |
| linearity | ||
| range (μg/mL) | 12.5–75.0 | 1.25–7.50 |
| slope | 48660 | 68462 |
| intercept | 12540 | 767.8 |
| correlation coefficient | 0.9997 | 0.9999 |
| precisiona | ||
| method precision (% RSD) | 0.7 | 0.5 |
| intermediate precision(%RSD) | 0.6 | 0.9 |
| accuracy (% recovery)b | ||
| 50% mean ± SD | 99.8 ± 0.3 | 99.2 ± 1.0 |
| 100% mean ± SD | 100.4 ± 0.4 | 99.6 ± 0.2 |
| 150% mean ± SD | 100.5 ± 0.3 | 99.9 ± 0.8 |
| solution stability | ||
| 24 h % assay difference with initial @ bench top | 0.5 | 0.3 |
| 24 h % assay difference with initial @ 2–8 °C | 0.9 | 0.8 |
Mean of six preparations.
Mean of triplicate preparations.
3.2.2. Forced Degradation Study
The combination of rRemogliflozin etabonate and teneligliptin was found to be sensitive to aAcid hydrolysis, alkali hydrolysis, peroxide conditions, and thermal conditions. No degradation was caused by light or neutral conditions. No interference or coelution of the peak with the analyte occurred. The method was specific, and the peak purity of the analyte peaks was passed through. Table 2 demonstrates the obtained result.
Table 2. Forced Degradation Summary Dataa.
| %assay of stressed samples | ||||
|---|---|---|---|---|
| nature of stress | condition | A | B | peak purity |
| unstressed | NA | 99.92 | 99.50 | purity angle less than purity threshold and no purity flag |
| acid | 2 N HCl@ 60 °C, for 30 min | 93.99 | 93.54 | |
| base | 2 N NaOH@60 °C, for 30 min | 95.18 | 95.01 | |
| peroxide | 20% H2O2@60 °C, for 30 min | 94.07 | 93.22 | |
| thermal | 105 °C for 6 h | 97.15 | 97.72 | |
| photostability | 7 days or 200 W h/min | 98.53 | 98.30 | |
| neutral | 60 °C for 6 h | 99.92 | 99.29 | |
A = remogliflozin. B= teneligliptin.
All chromatograms of forced degradation are displayed in Figures 3 and 4.
Figure 3.
Forced degradation study. Acid, base, and peroxide stress chromatograms.
Figure 4.
Forced degradation study. Thermal, photo, and neutral stress chromatograms.
3.2.3. Precision
Precision was carried out by preparing six test samples and analyzed as per the method. After analyzing the samples, the amount of analytes was calculated. Precision % RSD results for remogliflozin etabonate was 0.7%, and for teneligliptin, 0.5% was found. The obtained findings indicate the method’s confidence% RSD of less than 2.0%. Table 1 summarizes the findings.
Intermediate precision was accomplished by using different UPLCs with different columns and another analyst. The method was followed for the rest of the study. Samples with a precision and intermediate precision were computed. Remogliflozin etabonate’s method precision and intermediate precision were determined to be extremely low at 0.9 and 1.1%, respectively, for the % RSD of 12 spiking impurity samples. The results were consistent with the requirements. This demonstrates the method’s robustness. Table 1 summarizes the findings.
3.2.4. Stability of Analytical Solution
The stability of the standard and sample solutions was tested over time at room temperature and refrigerated temperatures. For the experiments, standard solutions and test sample solutions were made. The solutions were injected immediately after preparation. The solution was split in half, put into two volumetric flasks, and kept there for 24 h at both room temperature and a 2–8 °C refrigerator. After 24 h, the standard and sample solutions were both injected against freshly made standard solutions. We compared the differences between the initial and 24 h samples’ results. The results were acceptable, with a difference of less than 2.0% between the initial and 24 h results. The findings demonstrated that the standard and sample solutions remained stable for 24 h in both refrigerator and lab environments. In Table 1, results are displayed.
3.2.5. Linearity Study
The linearity of both analytes was tested between 50 and 150% (50, 80, 100, 120, and 150%) concentrations. To determine the slope, y-intercept, and correlation coefficient, triplicate injections of linear solutions were injected. Beer's law demonstrated that the analytes’ response was directly proportionate to concentration. Lambert’s correlation coefficient for both analytes was greater than 0.999. The slope and intercept were computed. The preceding results demonstrate that the method is linear. Table 1 summarizes the findings.
3.2.6. Accuracy
Recovery of analytes at levels between 50 and 150% was used to gauge the analytical method’s accuracy. Prepared sample solutions were at 50, 100, and 150% of the standard value. The samples were injected in triplicate in accordance with the method. Accuracy was demonstrated by the results of the method being similar to the actual values. The accuracy analysis ranged from 50 to 150%. Individual-level triplicate results ranged from a minimum of 98.1 to a maximum of 100.9%. These outcomes allow us to verify the method’s accuracy. Table 1 summarizes the findings.
3.2.7. Robustness
Using a QbD-based experimental tool design, the robustness parameters were determined. A two-stage, three-way interaction with three central points, consisting of two replicates and 19 experiments, was chosen. The factors A–C of the input technique were determined to be the flow rate (mL/min), mobile phase ratio (mL), and column oven temperature (°C), respectively. The resolution between both analytes was R1; the retention of remogliflozin etabonate was R2; and the retention time of teneligliptin was R3. Based on the real process conditions, the following changes are made to the input parameters. The flow rate was changed to 10% of what it was before (0.2 mL/min); the organic fraction was changed to 10% of what it was before (35:65 v/v); and the temperature of the column compartment was changed by 5 °C from what it was before (30 °C). Table 3 shows a summary of the DoE, with input values and output responses.
Table 3. Design of Experiments of Three Factors and Responsesa.
| factor 1 | factor 2 | factor 3 | response 1 | response 2 | response 3 | ||
|---|---|---|---|---|---|---|---|
| std | run | A: flow | B: organic ratio | C: column temp | R1 | R2 | R3 |
| 2 | 1 | 0.1 | 315 | 25 | 1.4 | 1.71 | 3.4 |
| 6 | 2 | 0.1 | 385 | 25 | 1.415 | 1.716 | 5.2 |
| 11 | 3 | 0.3 | 315 | 35 | 1.295 | 1.562 | 3.3 |
| 8 | 4 | 0.3 | 385 | 25 | 1.396 | 1.785 | 4.7 |
| 16 | 5 | 0.3 | 385 | 35 | 1.4 | 1.8 | 4.8 |
| 17 | 6 | 0.2 | 350 | 30 | 1.351 | 1.662 | 4.3 |
| 15 | 7 | 0.3 | 385 | 35 | 1.41 | 1.71 | 4.8 |
| 18 | 8 | 0.2 | 350 | 30 | 1.356 | 1.663 | 4.3 |
| 14 | 9 | 0.1 | 385 | 35 | 1.411 | 1.77 | 5.1 |
| 1 | 10 | 0.1 | 315 | 25 | 1.299 | 1.51 | 4.1 |
| 3 | 11 | 0.3 | 315 | 25 | 1.251 | 1.551 | 3.8 |
| 4 | 12 | 0.3 | 315 | 25 | 1.241 | 1.518 | 3.7 |
| 10 | 13 | 0.1 | 315 | 35 | 1.31 | 1.576 | 3.6 |
| 12 | 14 | 0.3 | 315 | 35 | 1.291 | 1.509 | 3.3 |
| 7 | 15 | 0.3 | 385 | 25 | 1.359 | 1.71 | 5.1 |
| 13 | 16 | 0.1 | 385 | 35 | 1.408 | 1.785 | 4.8 |
| 19 | 17 | 0.2 | 350 | 30 | 1.361 | 1.659 | 4.3 |
| 5 | 18 | 0.1 | 385 | 25 | 1.419 | 1.81 | 4.2 |
| 9 | 19 | 0.1 | 315 | 35 | 1.295 | 1.481 | 3.5 |
R1= retention time of remogliflozin. R2= retention time of teneligliptin. R3= resolution between remogliflozin and teneligliptin.
Seminormal plots were used to find significant effects in the DoE data through statistical analysis. The model is significant for all responses, but the lack of fit is not, as shown by the ANOVA data, suggesting that the design used is suitable for the current investigation. Table 4 provides a summary of the data from the DoE and the ANOVA.
Table 4. ANOVA Tablea.
| response | source | sum of squares | df | mean square | F-value | p-value | |
|---|---|---|---|---|---|---|---|
| R1 | model | 0.0541 | 4 | 0.0135 | 21.37 | <0.0001 | significant |
| A-flow | 0.0062 | 1 | 0.0062 | 9.74 | 0.0081 | ||
| B-organic ratio | 0.0437 | 1 | 0.0437 | 69.01 | <0.0001 | ||
| C-column temp | 0.0001 | 1 | 0.0001 | 0.158 | 0.6975 | ||
| AC | 0.0042 | 1 | 0.0042 | 6.57 | 0.0236 | ||
| curvature | 0.0001 | 1 | 0.0001 | 0.1437 | 0.7108 | ||
| residual | 0.0082 | 13 | 0.0006 | ||||
| lack of fit | 0.0022 | 3 | 0.0007 | 1.19 | 0.3635 | not significant | |
| pure error | 0.0061 | 10 | 0.0006 | ||||
| cor total | 0.0624 | 18 | |||||
| R2 | model | 0.1741 | 1 | 0.1741 | 58.23 | <0.0001 | significant |
| B-organic ratio | 0.1741 | 1 | 0.1741 | 58.23 | <0.0001 | ||
| curvature | 0.0001 | 1 | 0.0001 | 0.0203 | 0.8886 | ||
| residual | 0.0478 | 16 | 0.003 | ||||
| lack of fit | 0.01 | 6 | 0.0017 | 0.4392 | 0.8369 | not significant | |
| pure error | 0.0379 | 10 | 0.0038 | ||||
| cor total | 0.222 | 18 | |||||
| R3 | model | 6.25 | 1 | 6.25 | 81.47 | <0.0001 | significant |
| B-organic ratio | 6.25 | 1 | 6.25 | 81.47 | <0.0001 | ||
| curvature | 0.0193 | 1 | 0.0193 | 0.2521 | 0.6224 | ||
| residual | 1.23 | 16 | 0.0767 | ||||
| lack of fit | 0.3475 | 6 | 0.0579 | 0.6581 | 0.6851 | not significant | |
| pure error | 0.88 | 10 | 0.088 | ||||
| cor total | 7.5 | 18 |
R1= retention time of remogliflozin. R2= retention time of teneligliptin. R3= resolution between remogliflozin and teneligliptin.
Figure 5 depicts several different types of 3D plots, including a 3D cube plot, a 3D response surface plot, and a 2D half normal plot.
Figure 5.
Half normal plots, 2D contour plot, 3D plots, and 3D cube diagrams and for responses R1, R2, and R3.
Desirability plot and predicted plots for responses are shown in Figure 6. Figure 7 depicts overlay plots. The tailing factor, resolution, and number of plates used in each experiment were all within acceptable ranges.
Figure 6.
Desirability Plots and Predicted Plots for Responses R1, R2, and R3.
Figure 7.
Overlay plots for responses R1, R2, and R3.
3.2.8. Drug Product Analysis
In the final condition, the assay for three batches was determined once completing the validation activity to check the feasibility with the drug product, the results are found satisfactory, and the results are shown in Table 5.
Table 5. Analysis Results of the Three-Batch Assay for Both the Analytes.
| S. no. | batch | remogliflozin | teneligliptin |
|---|---|---|---|
| 1 | A | 99.8 | 100.1 |
| 2 | B | 99.6 | 99.8 |
| 3 | C | 99.7 | 99.8 |
4. Conclusions
The health care system places a premium on the reliability, consistency, and effectiveness of pharmaceutical formulations. In an oral solid formulation of remogliflozin etabonate and teneligliptin, quantity determination by the UPLC method was developed. It was found that the method is specific, exact, reproducible, rugged, accurate, linear, and robust after being validated in accordance with ICH Q2 (R1) and the USP general chapter. The stability sample analysis in shelf life studies benefited from the method’s stability-indicating nature, as shown by the forced degradation study. The proposed approach requires only limited validation studies before it can be employed in routine pharmaceutical quality control laboratories.
Acknowledgments
The authors are thankful to GITAM University for their support and guidance throughout the research.
The authors and institutions declare no financial interest or benefit from the work presented in this manuscript
The authors declare no competing financial interest.
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