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Supplementary material 1 from: Sharmin S, Sohrab MH, Moni F, Afroz F, Rony SR, Akhter S (2020) Simple RP-HPLC method for Aceclofenac quantitative analysis in pharmaceutical tablets. Pharmacia 67(4): 383-391. https://doi.org/10.3897/pharmacia.67.e57981
Table S1. HPLC Analytical methods for simultaneous estimation of Aceclofenac with other constituents
Factorial design assisted RP-HPLC method for simultaneous determination of fluconazole, itraconazole, and terbinafine
<p>A 2<sup>3</sup> full factorial design model was utilized for development of a new HPLC method with UV detection to estimate three antifungal drugs simultaneously. Fluconazole (FLU), itraconazole (ITR) and terbinafine (TRH), which are co-administered for severe fungal infections have been determined using MOS-1 Hypersil C18 column and an isocratic eluent; methanol 95% and phosphate buffer 5% with 0.001% triethylamine. The pH adjusted 7, and flow rate of 0.7 mL/min. The three drugs were separated within less than 7 minutes at 210 nm. The developed method gave linear response over 5-80, 5-50 and 1-50 μg/mL for FLU, ITR and TRH, respectively. It showed detection limits of 0.8761, 0.293 and 0.1965 μg/mL and quantification limits of 2.655, 0.8788 and 0.5956 μg/mL for the three drugs, respectively. The design of experiment facilitated the optimization of different variables affecting the separation of the three drugs. The designed method sensitivity permitted the simultaneous estimation of ITR and TRH in spiked human plasma successfully.</p>
Factorial design assisted RP-HPLC method for simultaneous determination of fluconazole, itraconazole, and terbinafine
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Figure 6 from: Sharmin S, Sohrab MH, Moni F, Afroz F, Rony SR, Akhter S (2020) Simple RP-HPLC method for Aceclofenac quantitative analysis in pharmaceutical tablets. Pharmacia 67(4): 383-391. https://doi.org/10.3897/pharmacia.67.e57981
Figure 6 Robustness Study (a) Variance of peak area for change in different method parameters with %RSD; (b) Variance of Retention time for change in different method parameters with %RSD. *Method was robust for change in pH of mobile phase (±0.5), wavelength (±3 nm) and column temperature (±3 °C).
Figure 4 from: Peikova L, Tzankova D, Dineva A, Georgieva M, Zlatkov A (2019) Development of a chiral RP-HPLC method for identification of stereomers of newly synthesized xanthine-based hydrazide-hydrazone compound. Pharmacia 66(1): 1-6. https://doi.org/10.3897/pharmacia.66.e35643
Figure 4 Representative chromatogram of the analyzed 2-(1,3-dimethyl-2,6-dioxo-2,3-dihydro-1H-purine-7(6H)-yl)-N'-(3-fluoro-benzylidene)propanehydrazide.
Figure 2 from: Peikova L, Tzankova D, Dineva A, Georgieva M, Zlatkov A (2019) Development of a chiral RP-HPLC method for identification of stereomers of newly synthesized xanthine-based hydrazide-hydrazone compound. Pharmacia 66(1): 1-6. https://doi.org/10.3897/pharmacia.66.e35643
Figure 2 A typical chromatogram of 2-(1,3-dimethyl-2,6-dioxo-2,3-dihydro-1H-purine-7(6H)-yl)-N'-(3-fluorobenzylidene)propanehydrazide racemate analysed using the final chromatographic conditions.
Figure 1 from: Peikova L, Tzankova D, Dineva A, Georgieva M, Zlatkov A (2019) Development of a chiral RP-HPLC method for identification of stereomers of newly synthesized xanthine-based hydrazide-hydrazone compound. Pharmacia 66(1): 1-6. https://doi.org/10.3897/pharmacia.66.e35643
Figure 1 Chemical structure of the evaluated 2-(1,3-dimethyl-2,6-dioxo-2,3-dihydro-1H-purine-7(6H)-yl)-N'-(3-fluorobenzylidene)propanehydrazide.
Figure 5 from: Tzankova D, Peikova L, Vladimirova S, Georgieva M (2019) Development and validation of RP-HPLC method for stability evaluation of model hydrazone, containing a pyrrole ring. Pharmacia 66(3): 127-134. https://doi.org/10.3897/pharmacia.66.e47035
Figure 5 Chromatogram of the separated mixture of the analyzed hydrazone D-5d (tR = 6.800) and its possible degradation products – the hydrazide D-5 (tR = 4.387) and the corresponding aldehyde d (tR = 1.387).
Figure 7 from: Tzankova D, Peikova L, Vladimirova S, Georgieva M (2019) Development and validation of RP-HPLC method for stability evaluation of model hydrazone, containing a pyrrole ring. Pharmacia 66(3): 127-134. https://doi.org/10.3897/pharmacia.66.e47035
Figure 7 Chromatograms indicating the behavior of D_5d in the presence of buffer with pH 2.0 and at 37°C at 0th min (A) and at 30th min (B).
Figure 4 from: Tzankova D, Peikova L, Vladimirova S, Georgieva M (2019) Development and validation of RP-HPLC method for stability evaluation of model hydrazone, containing a pyrrole ring. Pharmacia 66(3): 127-134. https://doi.org/10.3897/pharmacia.66.e47035
Figure 4 Chromatogram of standard solution of the aldehyde d (tR = 1.283) as possible degradation product.
Figure 3 from: Tzankova D, Peikova L, Vladimirova S, Georgieva M (2019) Development and validation of RP-HPLC method for stability evaluation of model hydrazone, containing a pyrrole ring. Pharmacia 66(3): 127-134. https://doi.org/10.3897/pharmacia.66.e47035
Figure 3 Chromatogram of standard solution of the hydrazide D-5 (tR = 4.380) as possible degradation product.
Figure 8 from: Tzankova D, Peikova L, Vladimirova S, Georgieva M (2019) Development and validation of RP-HPLC method for stability evaluation of model hydrazone, containing a pyrrole ring. Pharmacia 66(3): 127-134. https://doi.org/10.3897/pharmacia.66.e47035
Figure 8 Chromatograms indicating the behavior of D_5d in the presence of buffer with pH 9.0 and at 37°C at 0th min (A) and at 210th min (B).
Figure 9 from: Tzankova D, Peikova L, Vladimirova S, Georgieva M (2019) Development and validation of RP-HPLC method for stability evaluation of model hydrazone, containing a pyrrole ring. Pharmacia 66(3): 127-134. https://doi.org/10.3897/pharmacia.66.e47035
Figure 9 Chromatograms indicating the behavior of D_5d in the presence of buffer with pH 13.0 and at 37°C at 0th min (A) and at 30th min (B).
Figure 4 from: Sharmin S, Sohrab MH, Moni F, Afroz F, Rony SR, Akhter S (2020) Simple RP-HPLC method for Aceclofenac quantitative analysis in pharmaceutical tablets. Pharmacia 67(4): 383-391. https://doi.org/10.3897/pharmacia.67.e57981
Figure 4 Sensitivity Study.
Figure 3 from: Sharmin S, Sohrab MH, Moni F, Afroz F, Rony SR, Akhter S (2020) Simple RP-HPLC method for Aceclofenac quantitative analysis in pharmaceutical tablets. Pharmacia 67(4): 383-391. https://doi.org/10.3897/pharmacia.67.e57981
Figure 3 Calibration curve of linearity Study.
Figure 5 from: Sharmin S, Sohrab MH, Moni F, Afroz F, Rony SR, Akhter S (2020) Simple RP-HPLC method for Aceclofenac quantitative analysis in pharmaceutical tablets. Pharmacia 67(4): 383-391. https://doi.org/10.3897/pharmacia.67.e57981
Figure 5 Specifity study-response of the standard, sample, excipient and mobile phase.
Figure 2 from: Sharmin S, Sohrab MH, Moni F, Afroz F, Rony SR, Akhter S (2020) Simple RP-HPLC method for Aceclofenac quantitative analysis in pharmaceutical tablets. Pharmacia 67(4): 383-391. https://doi.org/10.3897/pharmacia.67.e57981
Figure 2 Absorbance maxima of Aceclofenac.
Figure 1 from: Sharmin S, Sohrab MH, Moni F, Afroz F, Rony SR, Akhter S (2020) Simple RP-HPLC method for Aceclofenac quantitative analysis in pharmaceutical tablets. Pharmacia 67(4): 383-391. https://doi.org/10.3897/pharmacia.67.e57981
Figure 1 Aceclofenac.
Figure 3 from: Tzankova D, Mateeva A, Mitkov J, Peikova L, Georgieva M (2022) Development and validation of RP-HPLC method for analytical characterization of the anabolic steroid Methenolone acetate in food supplements. Pharmacia 69(1): 151-155. https://doi.org/10.3897/pharmacia.69.e78176
Figure 3 Chromatogram of Methenolone standard solution.
Figure 2 from: Tzankova D, Mateeva A, Mitkov J, Peikova L, Georgieva M (2022) Development and validation of RP-HPLC method for analytical characterization of the anabolic steroid Methenolone acetate in food supplements. Pharmacia 69(1): 151-155. https://doi.org/10.3897/pharmacia.69.e78176
Figure 2 Linearity of the developed RP-HPLC method.
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