scholarly journals Quantitative Determination of Lercanidipine Enantiomers in Commercial Formulations by Capillary Electrophoresis

2015 ◽  
Vol 2015 ◽  
pp. 1-9 ◽  
Author(s):  
Luciana Pereira Lourenço ◽  
Fernando Armani Aguiar ◽  
Anderson Rodrigo Moraes de Oliveira ◽  
Cristiane Masetto de Gaitani
Keyword(s):  
Capillary Electrophoresis ◽  
Background Electrolyte ◽  
Pharmaceutical Formulations ◽  
Acetate Buffer Solution ◽  
Buffer Solution ◽  
Long Duration ◽  
Accuracy And Precision ◽  
Relative Errors ◽  
Optimum Separation

An enantioselective method based on capillary electrophoresis (CE) using cyclodextrin (CD) as chiral selector was developed and validated for determination of lercanidipine (LER) enantiomers, a drug calcium channel blocker which exerts antihypertensive effects of long duration, in a pharmaceutical formulation. Optimum separation of LER enantiomers was obtained on a 50 cm × 50 μm id capillary using a sodium acetate buffer solution 200 mmol/L pH 4.0 containing 10 mmol/L of 2,3,6-o-methyl-β-cyclodextrin (TM-β-CD) as background electrolyte. The capillary temperature and voltage were 15°C and 25 kV, respectively, hydrodynamic injection and detection at 237 nm. Linearity was obtained in the range 12.5–100 μg/mL for both enantiomers (r≥0.995). The RSD (%) and relative errors (E, %) obtained in precision and accuracy studies (intraday and interday) were lower than 5%. After validation, the method was applied to quantify the enantiomers of LER in commercial tablets and the results were satisfactory in terms of accuracy and precision, both less than 5%. Therefore, this method was found to be appropriate for enantioselective quality control of LER enantiomers in pharmaceutical formulations.

scholarly journals Electrochemically Activated Screen-Printed Carbon Electrode for Determination of Ibuprofen

2021 ◽  
Vol 11 (21) ◽  
pp. 9908
Author(s):  
Katarzyna Tyszczuk-Rotko ◽  
Jędrzej Kozak ◽  
Anna Węzińska
Keyword(s):  
Supporting Electrolyte ◽  
Pharmaceutical Formulations ◽  
Differential Pulse ◽  
Acetate Buffer Solution ◽  
Carbon Electrode ◽  
Buffer Solution ◽  
Screen Printed Carbon Electrode ◽  
Relative Errors ◽  
Screen Printed

In this study, we present a simple, sensitive and selective analytical procedure for the ibuprofen (IBP) analysis using the commercially available screen-printed carbon electrode electrochemically activated (aSPCE) by cyclic voltammetry in 0.1 M NaOH. The quantitative determinations of IBP were carried out in 0.25 M acetate buffer solution of pH 4.5 ± 0.1 using the differential-pulse voltammetry (DPV). Different experimental parameters for DPV analysis were optimized, including pH and concentration of supporting electrolyte, amplitude (ΔEA), scan rate (ν) and modulation time (tm). The linear ranges of calibration curve were from 0.50–20.0 and 20.0–500.0 µM. The detection and quantification limits were estimated to be 0.059 and 0.20 µM. The aSPCE displayed satisfactory repeatability, reproducibility, and selectivity. Furthermore, the DPV procedure with the use of aSPCE was used to determination of IBP in pharmaceutical formulations. The results achieved by DPV show satisfactory agreement with those obtained by manufacturers (the relative errors are in the range of 3.1–4.7%).

scholarly journals Spectrophotometric Determination of Pipazethate Hydrochloride in Pure Form and in Pharmaceutical Formulations

2007 ◽  
Vol 90 (3) ◽  
pp. 686-692 ◽  
Author(s):  
Ragaa El-Shiekh ◽  
Alaa S Amin ◽  
Faten Zahran ◽  
Ayman A Gouda
Keyword(s):  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Pure Form ◽  
Acetate Buffer Solution ◽  
Buffer Solution ◽  
Accurate Analysis ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Optimum Ph

Abstract Three simple, sensitive, and reproducible spectrophotometric methods (AC) for the determination of pipazethate hydrochloride (PiCl) in pure form and in pharmaceutical formulations are described. The first and second methods, A and B, are based on the oxidation of the drug by Fe3+ in the presence of o-phenanthroline (o-phen) or bipyridyl (bipy). The formation of tris-complex upon reactions with Fe3+-o-phen and/or Fe3+-bipy mixture in an acetate buffer solution of the optimum pH values was demonstrated at 510 and 522 nm, respectively, with o-phen and bipy. The third method, C, is based on the reduction of Fe(III) by PiCl in acid medium and subsequent interaction of Fe(II) with ferricyanide to form Prussian blue, which exhibits an absorption maximum at 750 nm. The concentration ranges are from 0.5 to 8, 2 to 16, and 3 to 15 g/mL for Methods AC, respectively. For more accurate analysis, Ringbom optimum concentration ranges were calculated. The molar absorptivity, Sandell sensitivity, and detection and quantitation limits were calculated. The developed methods were successfully applied to the determination of PiCl in bulk and pharmaceutical formulations without any interference from common excipients. The relative standard deviations were 0.83% with recoveries of 98.9101.15%.

scholarly journals Method Validation for Determination of Metformin Hydrochloride in Pharmaceutical Formulations by Capillary Electrophoresis with Capacitively Coupled Contactless Conductivity Detection

2019 ◽  
pp. 1-10
Author(s):  
Gazala Mohamed Ben-Hander ◽  
Ashraf Ahmed Ali Abdusalam ◽  
Bahruddin Saad ◽  
Ahmad Makahleh ◽  
Salizawati Muhamad Salhimi
Keyword(s):  
Capillary Electrophoresis ◽  
Background Electrolyte ◽  
Pharmaceutical Formulations ◽  
Fused Silica ◽  
Metformin Hydrochloride ◽  
Capacitively Coupled ◽  
Fused Silica Capillary ◽  
Normal Polarity ◽  
C 30

A method for the determination of metformin hydrochloride (MH) in pharmaceutical formulations by capillary electrophoresis with capacitively coupled contactless conductivity (C4D) detection was investigated. The separation was achieved under normal polarity mode at 17.5°C, 30 kV, hydrodynamic injection (50 mbar for 8 s) and using a bare fused silica capillary 72 cm × 75 µm i.d. (detection length, 10.5 cm from the outlet end of the capillary). The optimized background electrolyte consisted of 10 mM 2-morpholinoethanesulfonic acid and 10 mM histidine, pH 6.8. C4D parameters were set at fixed amplitude of 100 V and frequency of 650 kHz. Under the optimum conditions, the method shows good linearity over the range of 10-30 µg mL-1 MH (r2=0.9971). Limits of detection and quantitation based on S/N ratio of 3 and 10 were 0.049 and 0.15 µg mL-1, respectively. The proposed method was successfully applied to the assay of MH in pharmaceutical formulations and establishing the dissolution profiles for both immediate and extended release formulations of MH.

Comparative Study for the Assay of Plant Derived Chemicals in Pharmaceutical Formulation Using Methods Dependent on Factorized Spectra

2021 ◽  
Author(s):  
Nesma M Fahmy ◽  
Adel M Michael
Keyword(s):  
Pharmaceutical Formulations ◽  
Pharmaceutical Formulation ◽  
Ternary Mixtures ◽  
Ratio Method ◽  
The Novel ◽  
Naturally Occurring ◽  
Accuracy And Precision ◽  
Validation Parameters ◽  
Significant Difference

Abstract Background Modern built-in spectrophotometer software supporting mathematical processes provided a solution for increasing selectivity for multicomponent mixtures. Objective Simultaneous spectrophotometric determination of the three naturally occurring antioxidants—rutin(RUT), hesperidin(HES), and ascorbic acid(ASC)—in bulk forms and combined pharmaceutical formulation. Method This was achieved by factorized zero order method (FZM), factorized derivative method (FD1M), and factorized derivative ratio method (FDRM), coupled with spectrum subtraction(SS). Results Mathematical filtration techniques allowed each component to be obtained separately in either its zero, first, or derivative ratio form, allowing the resolution of spectra typical to the pure components present in Vitamin C Forte® tablets. The proposed methods were applied over a concentration range of 2–50, 2–30, and 10–100 µg/mL for RUT, HES, and ASC, respectively. Conclusions Recent methods for the analysis of binary mixtures, FZM and FD1M, were successfully applied for the analysis of ternary mixtures and compared to the novel FDRM. All were revealed to be specific and sensitive with successful application on pharmaceutical formulations. Validation parameters were evaluated in accordance with the International Conference on Harmonization guidelines. Statistical results were satisfactory, revealing no significant difference regarding accuracy and precision. Highlights Factorized methods enabled the resolution of spectra identical to those of pure drugs present in mixtures. Overlapped spectra of ternary mixtures could be resolved by spectrum subtraction coupled FDRM (SS-FDRM) or by successive application of FZM and FD1M.

Polarographic Determination of Zinc in Compounded Rubber

1950 ◽  
Vol 23 (4) ◽  
pp. 975-980
Author(s):  
F. C. J. Poulton ◽  
L. Tarrant
Keyword(s):  
Zinc Oxide ◽  
Ammonium Acetate ◽  
Potassium Thiocyanate ◽  
Acetate Buffer Solution ◽  
Acid Electrolyte ◽  
Buffer Solution ◽  
Ammonium Acetate Buffer ◽  
Ammonium Acetate Buffer Solution ◽  
Gravimetric Procedure

Abstract Reasons are advanced for the unsatisfactory nature of some of the older methods for the determination of very small amounts of zinc in compounded rubber, particularly in latex mixings. The polarographic technique offers a possible solution, but most of the commoner electrolytes for the electroreduction of this metal are alkaline, and give rise to similar errors as are met in the gravimetric procedure. The development of a suitable acid electrolyte was therefore undertaken, and ways of dealing with likely interferences were examined. The electroltye finally recommended is a potassium thiocyanate-ammonium acetate buffer solution; iron, when present, is reduced to the ferrous condition by potassium iodide. The method was used to determine zinc oxide in a series of mixings of known composition ranging from 0.8 to 40 per cent. In all except the highest proportions of zinc oxide, the figures obtained agree well with the theoretical.

The use of photogenerated iodine in determination of the dibazol content in solid and liquid dosage formulations

2021 ◽  
Vol 87 (2) ◽  
pp. 19-24
Author(s):  
E. V. Turusova
Keyword(s):  
Generation Time ◽  
Quantitative Estimation ◽  
Potato Starch ◽  
Analytical Signal ◽  
Acetate Buffer Solution ◽  
Molar Ratio ◽  
Buffer Solution ◽  
Solution Ph ◽  
Solid Dosage

A rapid method for the determination of Dibazol (bendazol hydrochloride) in liquid and solid dosage forms (DF) has been developed. The method is based on converting the drug into an analytical form and titrating the physiologically active compound (PAC) with a solution of photogenerated iodine obtained by irradiation of an auxiliary solution containing potassium iodide, a mixture of sensitizers (sodium eosinate: fluorescein: auramine, taken in a molar ratio of 1:1:1) and an acetate buffer solution (pH 5.6). A decrease in the titrant content in the cell due to interaction with Dibazol was recorded by a decrease in the current in the amperometric circuit. Stabilization of the current in the circuit indicated the completeness of the reaction, thus providing for estimation of the PAC content in a DF. Further irradiation of the solution and measurement of the generation time required to replenish the titrant loss in the cell also ensure the quantitative estimation of the PAC content in the preparation. The method has been tested on solid dosage form and sterile solutions of Dibazol intended for intramuscular and intravenous administration. A slight effect of stabilizers (hydrochloric acid, ethanol) and auxiliary substances (potato starch) present in the DF on the photogeneration of the titrant was observed. The determined Dibazol content in solid and liquid DF falls within the range recommended by the order of the Ministry of Health of the Russian Federation (26.10.2015 No. 751n) and OFS.1.4.2.0009.15, which indicates that the quality of the drug meets the GMP standards. The linear dependence of the analytical signal on the Dibazol concentration is observed in the range of 13.5 – 134.7 mg for the drug «Dibazol-UBF, tablets, 20 mg». The calculated limits of Dibazol detection and quantitative determination by changes in the current strength and generation time are (4.71; 3.56) and (14.26; 10.77) mg, respectively. The use of developed technique in the analysis of drugs containing Dibazol reduces both the time of single determination due to the absence of the need for standardization of solutions, and the cost of a single analysis, since it does not require the use of expensive equipment and reagents.

Determination of Ofloxacin Enantiomers in Pharmaceutical Formulations by Capillary Electrophoresis

2007 ◽  
Vol 31 (3) ◽  
pp. 348-360 ◽  
Author(s):  
Abdalla A. Elbashir ◽  
Bahruddin Saad ◽  
Abdussalam Salhin Mohamed Ali ◽  
Muhammad Idiris Saleh ◽  
Hassan Y. Aboul‐Enein
Keyword(s):  
Capillary Electrophoresis ◽  
Pharmaceutical Formulations ◽  
Ofloxacin Enantiomers
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