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    Flow-injection chemiluminescence determination of aminoglycoside antibiotics using N-bromosuccinimide-fluorescein system
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    Abstract:
    A flow-injection chemiluminescence method for the determination of tobramycin, micro-nomicin, amikacin and gentamycin has been described. The method utilises chemiluminescence ofthe above analytes emitted during their oxidation with N-bromosuccinimide (NBS) in alkaline medium in the presence of fluorescein. The obtained detection limits (3σ) are 0.07 μg mL - 1 for tobramycin and 0.08 μg mL - 1 for micronomicin, amikacin and gentamycin. The evaluated method is recommended for automated and continuous analysis. In the automated mode the samples can be analysed at the rate of 100 per h with RSD of about 2.0% for the determination of 5 μg mL - 1 of each aminoglycoside antibiotic (n = 11). The proposed method has been successfully used for the analysis of commercial pharmaceutical formulations without any sample pretreatment.
    Keywords:
    Amikacin
    N-Bromosuccinimide
    Flow injection analysis
    A simple and rapid capillary zone electrophoretic (CZE) method has been established for separation and quantification of a mixture of eight cephalosporins – cefadroxil (CFL), cefixime (CIX), cefuroxime sodium (CFR), ceftriaxone sodium (CTR), ceftizoxime (CFT), cefaclor (CFC), cefradine (CFD), and cefotoxime (CTA). Conditions affecting the separation were pH, buffer concentration, and applied potential. Separation was performed in less than 11 min with 50 mM sodium tetraborate buffer, pH 9.0, and an applied potential of 30 kV. Reproducible separation was achieved and calibration plots were linear over two to three orders of magnitude of analyte concentration. Limits of detection were in the range 0.5–5 µg mL –1 . Detection was by UV absorbance at 214 nm. When the method was assessed for analysis of cephalosporins in pharmaceutical preparations and in urine, relative standard deviations (RSD, n = 4) were in the range 0.3–1.9%.
    Cefixime
    Cefadroxil
    Ceftizoxime
    Cefaclor
    Quantitative Analysis
    Cephalosporin Antibiotic
    Absorbance
    Cephradine
    Citations (13)
    Objective To develop a satisfactory and reliable method for simultaneous determination of seven cephalosporin antibiotics (cefadroxil,cephalexin,cefoperazone,cefuroxime,cefradine,ceftazidime and cefotaxime) in water samples using solidphase extraction and high performance liquid chromatography.Methods The detection and reference wavelengths were 254 and 270 nm,respectively.The analytes were separated within 20 min by a gradient elution program.The optimized pretreatment of water samples was as following:using hydrophilic-lipophilic balance HLB as SPE cartridges,adjusting pH to 3 and adding 3.0 g NaCl per 500 ml water sample.Results The linear range of the method was 0.05-5.00 mg/L for ceftazidime,cefotaxime and cefuroxime,0.10-10.00 mg/L for cefadroxil,cephalexin and cefradine,and 0.20-20.00mg/L for cefoperazone.The coefficients for the analytes were above 0.99 and the limits of determination were 0.05-0.39 μg/L.The recoveries of seven cephalosporin antibiotics in purified water were 86.64%-105.28%,and its relative standard deviation were 2.61%-11.64%.Conclusion The method was sensitive,accurate and repeatable,it is applicable to the determination of the cephalosporin antibiotics in waters.
    Cefadroxil
    Cefuroxime
    Cefoperazone
    Cephalosporin Antibiotic
    Citations (0)
    A simple, accurate, and specific liquid chromatographic procedure is described for the determination of gentamicin in 50 µL of serum. Gentamicin and sisomicin (IS) were converted into their trinitrophenyl derivatives by reaction with a water soluble derivatizing agent at 70°C for 30 minutes. The derivatives were extracted from the crude mixture with chloroform, which was separated, evaporated, and the residue reconstituted in acetonitrlle. Gentamicin was separated Into three major isomers (C1, C2, and C1) on a reversed-phase octyl column by eluting with a mobile phase. The eluted compounds were detected at 340 nm and quantified from their peak heights or peak areas. Chromatography was complete in ◂11.0 minutes. The lower limit of detection for gentamicin was ◂0.5 mg/L, analytical recoveries varied from 96.6% to 99.3%, linearity extended to 15.0 rag/L, and day-to-day precision was between 2.2% to 2.9%.
    Sisomicin
    Residue (chemistry)
    Citations (5)
    The quantitative estimation of amikacin (AMK) in AMK sulfate injection samples is reported using FTIR-derivative spectrometric method in a continuous flow system. Fourier transform of mid-IR spectra were recorded without any sample pretreatment. A good linear calibration (r>0.999, %RSD<2.0) in the range of 7.7-77.0 mg/mL was found. The results showed a good correlation with the manufacturer's and overall they all fell within acceptable limits of most pharmacopoeial monographs on AMK sulfate.
    Amikacin
    Derivative (finance)
    Citations (13)
    Objective:To estabilish a ion chromatography method for determination of the related substances in amikacin sulfate raw materials and its preparations.Methods:An Carbopac MA1(250 mm×4 mm)column was used with the eluent of deionized water(A) and 400 mmol·L-1 sodium hydroxide solution(B),the flow rate was 0.4 mL·min-1,the column temperature was 35 ℃.Amperometric detector,working electrode was gold electrode(1 mm).Results:The linear rang of amikacin was 0.9-4.8 μg·mL-1(r=0.9994),and the linear rang of amikacin impurity A was 1.0-8.1 μg·mL-1(r=0.9994).The precisions(RSD) of amikacin and amikacin impurity A were 1.8% and 1.9%,the detection limits were 3.6 ng and 3.2 ng respectively.The sample solution was stable within 10 h.Conclusion:This method was simple,sensitive and can be applied for the related substances of amikacin raw materials and its preparations.
    Amikacin
    Sodium hydroxide
    Ion chromatography
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