Current Issue : October - December Volume : 2020 Issue Number : 4 Articles : 6 Articles
Green analytical technologies for the determination of a bioactive compound diosmin\n(DIOM) in the real samples of pharmaceutical formulations and biological fluids are scarce in literature.\nTherefore, the present investigation was carried out to develop a novel, rapid, simple, and economical\ngreen â??reversed phase high-performance thin-layer chromatography (RP-HPTLC)â? method for the\ndetermination of DIOM in commercial tablets and in-house developed spray-dried microparticles\n(MPs). The quantification of DIOM was conducted via â??RP-18 silica gel 60 F254S HPTLC platesâ?.\nThe binary combination of green solvents, i.e., ethanol:water (5.5:4.5 v/v) was proposed as a green\nmobile phase. The analysis of DIOM was conducted in absorbance/reflectance mode of densitometry\nat Lmax = 348 nm. The densitograms of DIOM from the commercial tablets and in-house developed\nspray-dried MPs were verified by recording their single band at Rf = 0.80 0.02 compared to\nstandard DIOM. Green RP-HPTLC method was observed as linear in the range of 100â??700 ng/band\nwith R2 = 0.9995. The proposed method was found as â??accurate, precise, robust, and sensitiveâ?\nfor the determination of DIOM in the real samples of commercial tablets and in-house developed\nspray-dried MPs. The % content of DIOM in the real samples of commercial tablets and in-house\ndeveloped spray-dried MPs was obtained as 99.06 and 101.30%, respectively. The recorded results\nof this research suggested that the green RP-HPTLC method can be eectively used for the routine\nanalysis of DIOM in pharmaceutical products....
Developed methods for routine analysis of medicines should be considered in terms of\nanalytical effciency, economic cost, as well as their environmental impact. Different chromatographic\nmethods for the routine quantitative analysis of hederacoside C in ivy leaf extract and its original\ndosage forms (capsules and syrup) are developed. The performance of HPLC and UPLC methods\nshould be done using ACE C18 (150 mm x 4.6 mm, 5.0 microM) and ACQUITY UPLC BEH C18\n(50 mm x 2.1 mm, 1.7 microM) columns, respectively, and both of them require a mixture of water\nand acetonitrile in the ratio 71/29 as a mobile phase. The HPTLC procedure is carried out using\nthe stationary phase pre-coated silica gel 60 F254 glass sheets and a mixture of anhydrous formic\nacid/acetone/methanol/ethyl acetate (4:20:20:30 v/v). The most suitable conditions of preparation\nfor each sample are established, for instance, the solid-phase extraction (SPE) for the analysis of\nsyrup is applied. Analytical methods are compered by analytical accuracy, calculation of expenses,\nand assessment of their influence on ecology. All methods are recognized as accurate, precise,\nand reliable. However, the assessment of the environmental impact shows that HPTLC is the less\ngreen method. On the another hand, it is found to be the cheapest, the costs of performing HPTLC\nare 2.3 and 1.6 times lower than for HPLC and UPLC, respectively....
Alkaline hydrogen peroxide oxidation (AHPO) of eumelanin and pheomelanin,\ntwo major classes of melanin pigments, affords pyrrole-2,3,5-tricarboxylic acid (PTCA), pyrrole-2,3-\ndicarboxylic acid (PDCA) and pyrrole-2,3,4,5-tetracarboxylic acid (PTeCA) from eumelanin and\nthiazole-2,4,5-tricarboxylic acid (TTCA) and thiazole-4,5-dicarboxylic acid (TDCA) from pheomelanin.\nQuantification of these five markers by HPLC provides useful information on the quantity and\nstructural diversity of melanins in various biological samples. HPLC analysis of these markers\nusing the original method of 0.1 M potassium phosphate buffer (pH 2.1):methanol = 99:1 (85:15 for\nPTeCA) on a reversed-phase column had some problems, including the short lifetime of the column\nand, except for the major eumelanin marker PTCA, other markers were occasionally overlapped by\ninterfering peaks in samples containing only trace levels of these markers. These problems can be\novercome by the addition of an ion pair reagent for anions, such as tetra-n-butylammonium bromide\n(1 mM), to retard the elution of di-, tri- and tetra-carboxylic acids. The methanol concentration was\nincreased to 17% (30% for PTeCA) and the linearity, reproducibility, and recovery of the markers\nwith this improved method is good to excellent. This improved HPLC method was compared to the\noriginal method using synthetic melanins, mouse hair, human hair, and human epidermal samples.\nIn addition to PTCA, TTCA, a major marker for pheomelanin, showed excellent correlations between\nboth HPLC methods. The other markers showed an attenuation of the interfering peaks with the\nimproved method. We recommend this improved HPLC method for the quantitative analysis of\nmelanin markers following AHPO because of its simplicity, accuracy, and reproducibility....
Solid dispersions were prepared via a solvent evaporation method, employing ethanol\n(96%, v/v) as solvent, with three different polymers as carrier: povidone, copovidone, and poloxamer\n407. Previously developed reversed-phase HPLC (RP-HPLC) methods were modified and used for\nthe simultaneous determination of acetylsalicylic acid and clopidogrel bisulfate and after release\nfrom solid dispersions. Chromatography was carried out on a C-18 column, with a mobile phase of\nacetonitrileâ??methanolâ??phosphate buffer pH 3.0, UV detection at 240 nm, and a run time of 6 min.\nThe method was validated according to International Conference of Harmonisation guidelines and\nvalidation included specificity, accuracy, precision, linearity, robustness, limit of detection (LOD),\nand limit of quantification (LOQ). The method is specific for determination of acetylsalicylic acid and\nclopidogrel bisulfate. The linearity was provided in the concentration range 0.0275â??0.1375 mg/mL\nfor acetylsalicylic acid and 0.0200â??0.1000 mg/mL for clopidogrel bisulfate, with a correlation\ncoeffcient (R2 value) of 0.9999 for both active pharmaceutical ingredients (APIs). Accuracy was\nconfirmed by calculated recoveries for acetylsalicylic acid (98.6â??101.0%) and clopidogrel bisulfate\n(100.0â??101.6%). The intra-day and the inter-day precision-calculated relative standard deviations\nare less than 1%, which indicates high precision of the method. The limits of detection and\nquantification for acetylsalicylic acid were 0.0004 and 0.0012 mg/mL, and for clopidogrel bisulfate\n0.0002 mg/mL and 0.0007 mg/mL, respectively. Small variations in chromatographic conditions did\nnot significantly affect qualitative and quantitative system responses, which proved robustness of\nmethod. The proposed RP-HPLC method was applied for simultaneous determination of clopidogrel\nbisulfate and acetylsalicylic acid from solid dispersions....
A simple, Accurate, precise method was developed for the simultaneous estimation of the ivabradine and metoprolol in tablet dosage form. Chromatogram was run through Agilent C18 150 x 4.6 mm, 5m. Mobile phase containing Methanol:KH2PO4 taken in the ratio 50:50 was pumped through column at a flow rate of 0.8 ml/min. Temperature was maintained at 30°C. Optimized wavelength selected was 260.0 nm. Retention time of metoprolol and ivabradine were found to be 2.210 min and 2.650 min. %RSD of the ivabradine and metoprolol were and found to be 0.4 and 0.6 respectively. %Recovery was obtained as 99.89% and 100.09% for ivabradine and metoprolol respectively. LOD, LOQ values obtained from regression equations of ivabradine and metoprolol were 0.02, 0.06 and 0.24, 0.74 respectively. Regression equation of ivabradine is y = 33598x + 1032 and y = 43436x + 2674 of metoprolol. Retention times were decreased and that run time was decreased, so the method developed was simple and economical that can be adopted in regular quality control test in industries....
A simple, economic and accurate method was developed for the simultaneous determination of clotrimazole and lignocaine HCl in ear drops by RP-HPLC. Chromatographic separation of the drugs, achieved on Hypersil C-18 (250×4.6 mm, 5μ) column at 225 nm, mobile phase comprising a mixture of methanol-buffer in the ratio of 90:10 v/v, at a flow rate of 1.1 mL/min. Lignocaine HCl and clotrimazole were eluted at 3.382 and 4.2 mins respectively. Calibration curves were linear over the range of 10-250 μg/ml, 10-300 μg/ml for clotrimazole and lignocaine HCl with r2 values, 0.997 and 0.999 respectively. The % assay of clotrimazole and lignocaine HCl were 99.6 and 98.98% respectively. The performance of the method was validated according to ICH guidelines. The proposed method was successfully applied for the determination of clotrimazole and lignocaine HCl in ear drops. The performance of the method was validated according to ICH guidelines....
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