Chemiluminescence determination of amikacin based on the inhibition of the luminol reaction catalyzed by copper (original) (raw)
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Journal of the Chemical Society of Pakistan, 2016
Amikacin sulphate is devoid of any chromophore and/or conjugated system prerequisite for UV and florescent light detection (FLD). Hence, there is a need of simple and reliable methods for introducing chromophore in the structure of amikacin sulphate for its determination using UV and FLD. Therefore, the present study describes the development and validation of a simple, economical and fast colorimetric method for estimation of the drug. The analyte and aqueous ninhydrin solution upon heating for 2-5 min produced the Ruhemann purple colored drug-derivative which was detected at two wavelengths, 400 nm and 567 nm. Beer’s law was obeyed over the concentration ranges from 0.417 mg/ml to 2.500 mg/ml. The method was found to be reliable (95.07 – 100.52 % recovery at 400 nm and 96.04 – 99.89 % at 567 nm), repeatable intraday accuracy (95.07 – 100.52 % at 400 nm and 96.04 – 99.84 % at 567 nm) and reproducible -inter day accuracy (95.25– 99.91 % at 400 nm 96.52 – 99.89 % at 567 nm) with rela...
Pharmaceutical methods, 2016
Background: Amikacin belongs to aminoglycosides family, commonly administered in the treatment of systemic infections due to gram negative bacteria. Its narrow therapeutic index results in adverse effects like nephrotoxicity and ototoxicity. Objective: Optimize an ultra-high performance liquid chromatography (UHPLC) based analytical method for the determination of amikacin sulfate in human serum using derivatizaon with FMOCCl and glycine. Methods: Pre-column derivatization reaction of amikacin performed using fluorescence reagent 9-fluorenylmethyl chloroformate (FMOC-Cl) at ambient temperature in the presence of borate buffer (0.2 M). Stabilizing reagent glycine (0.1 M) added into the reaction mixture solution after completion of the derivatization reaction for stabilization of fluorescent complex product. Fluorimetric detection of amikacin was performed at excitation and emission wavelength of 265 nm and 315 nm respectively, using C18 UHPLC column. The reported method was validated...
A Recent Review on Chemiluminescence Reaction, Principle and Application on Pharmaceutical Analysis
ISRN Spectroscopy, 2013
This paper provides a general review on principle of chemiluminescent reactions and their recent applications in drug analysis. The structural requirements for chemiluminescent reactions and the different factors that affect the efficiency of analysis are included in the review. Chemiluminescence application in immunoassay is the new version for this review. Practical considerations are not included in the review since the main interest is to state, through the aforementioned applications, that chemiluminescence has been, is, and will be a versatile tool for pharmaceutical analysis in future years.
Journal of the Iranian Chemical Society
Amikacin (AMK) is an important member of aminoglycoside class, and its determination has therapeutic importance due to its matchless potency against gram -ve pathogens. Due to narrow therapeutic window, its monitoring in clinical samples is inevitable. Direct determination of AMK using HPLC with UV-visible detection is not possible because of its limited absorbance. Herein, Hantzsch reagent (mixture of acetylacetone, formaldehyde and acetate buffer) was used as pre-column derivatization for AMK. UV-visible detection was performed at 340 nm. Separation and identification of derivatized drug (amikacin) were carried out using C-18 column Kromasil 100 (15 cm × 0.46 mm, 5 μm) with isocratic mobile phase elution of pH 5 (acetate buffer 0.01 M):acetonitrile (30:70 v/v) with flow rate of 1 ml/min. The procedure was able to resolve AMK from endogenous compounds and from cephalosporin drug (most prescribed combination) with run time of 10 min. Under optimized conditions; calibration curve was linear in the range 0.10-25.0 µg/mL with LOD and LOQ values of 0.024 and 0.071 µg/mL. Method was also validated for reproducibility, ruggedness and accuracy. The procedure was found sensitive, robust and precise for the comprehensive analysis (qualitative and quantitative) that was applied for determination of AMK in pharmaceuticals, urine and blood samples.
Rasayan Journal of Chemistry, 2020
Amikacin is an antibiotic worn in the treatment of bacterial infectious diseases. An easy chromatographic technique was evaluated for the fortitude of the related compound. Newly improved method attained through isocratic elution on X bridge C18 (250 x 4.6 mm, 5µm) column at 30 °C using a mobile phase consisting of phosphate buffer and methanol (70:30 v/v) with a flow rate of 1.0 mL/min. The UV detection was carried at 340 nm. The analytical execution of the new method was validated as per International Council for Harmonization (ICH)
Luminescence, 2011
ABSTRACTA highly selective and simple chemiluminescence (CL) method for determination of penicillin G potassium (PGK) was developed. In the proposed method, CL was elicited from PGK upon its oxidation with H2O2. The light emission was enhanced in the presence of N‐cetyl‐N,N,N‐trimethylammonium bromide (CTMAB). An experimental design, central composite design (CCD), was used to realize the optimized variables, including pH, surfactant (CTMAB) and H2O2 concentrations. Under optimum condition, the calibration graph was linear in the range 3.3 × 10−3–3.3 × 10−1 mmol/L, with a detection limit of 8.8 × 10−4 mmol/L for PGK. The precision was calculated by analysing samples containing 1.6 × 10−1 mmol/L PGK (n = 5) and the relative standard deviation (RSD) was 1.40%. The utility of this method was demonstrated by determining PGK in pharmaceutical formulations for injection. The proposed method was validated by a reference method. Copyright © 2011 John Wiley & Sons, Ltd.
Journal of Young Pharmacists, 2015
Objective: To determine the amikacin sulfate by developing a new spectrophotometric method by derivatization using double beam spectrophotometer from pure and commercial brands. Method: A quantitative analytical method was developed by amikacin sulfate using spectrophotometer after derivatization with vanillin under optimized parameters like pH, heating time and temperature, volume of reagent, Impact of mixing order, Effect of addition of solvents and Effect of excipients. The method was successfully applied on bulk and different brands containing amikacin sulfate. Results: The bulk and pharmaceutical analysis was carried out of different brands with formation of slight yellow colored imine base. The product showed absorbance at 400 nm w i t h molar absorptivity of 5.27x10 3 L/mole/ cm. In a concentration of 10-50 µg ml-1 a linear relationship was established w i t h absorbance which follow the beer's law with coefficient of determination r 2 0.9991-0.9998. The procedure was valid because it did not show change in absorbance of the derivative up to 3 days. The sandells sensitivity was calculated as 0.004 at 0.45 µg mL-1 of amikacin sulfate with vanillin. The percentage of recovery was 103-106.4% with RSD of 0.004-0.005.
Liquid Chromatographic Determination of Amikacin Sulphate after Pre-Column Derivatization
Journal of Chromatographic Science, 2013
A novel high performance liquid chromatographic (HPLC) method with a pre-column derivatization reaction has been developed and validated. The method was used for the determination of the aminoglycoside antibiotic amikacin sulphate (AMK) in the presence of its synthetic precursor kanamycin sulphate in pure form and in different pharmaceutical preparations. The pre-column derivatization was based on Hantzsch condensation reaction and the obtained coloured products were separated using an isocratic reversed-phase high performance liquid chromatographic method. The separation was achieved on a Spherisorb C18 ODS2 (250 3 4.6 mm, 5 mm) column using a mobile phase composed of acetonitrile -0.1 M sodium acetate buffer ( pH 5.0; 25:75, v/v). The column temperature was adjusted at 358 8 8 8 8C and the flow rate at 2 mL min 21 . The detection was carried out at 330 nm by using photo-diode array detector. Different conditions for the optimization of the derivatization reaction as well as for the HPLC measurement were studied. Moreover, AMK was subjected to forced degradation by oxidation, hydrolysis, photolysis and dry heat. Degradation products did not interfere with the assay, which can thus be considered selective and specific. The proposed method was validated for linearity, precision, accuracy, specificity and robustness. Also, it was used to check the purity of AMK in the presence of KAN (related impurity) at the pharmacopoeial limit (0.5%).
Analytica Chimica Acta, 2010
In this work, both the batch and flow injection chemiluminescence (CL) methods have been proposed for the simultaneous determination of two structurally similar -lactams including amoxicillin and clavulanic acid (CLAV). Chemiluminescence spectral overlap of these two structurally similar -lactams is the main limitation for the simultaneous analysis of the two compounds. Least squares support vector regression (LS-SVR) was applied to relate concentration of both the compounds to their CL profiles. The parameters of the model, consisting of kernel parameter, 2 , and the regularization parameter, , were optimized by constructing different LS-SVR models and the model with the minimum root mean squared error of cross-validation (RMSECV) for the calibration set was selected as the best model and its parameters were chosen as the optimized values. The performance of LS-SVR model was compared with Partial Least Squares (PLS) and the results revealed the superiority of the LS-SVR over PLS model. Under the optimized experimental conditions for both the compounds, when LS-SVR was applied, the detection limits obtained were 0.2 and 0.60 mol L −1 in the batch mode and 0.3 and 0.5 mol L −1 in the flow injection mode for CLAV and amoxicillin, respectively. The proposed method was utilized for the simultaneous determination of the compounds in pharmaceutical formulations and spiked plasma samples.