Method For Determination Of Ciprofloxacin Research Articles

Simple, fast and reliable CE method for simultaneous determination of ciprofloxacin and ofloxacin in human urine

A simple, fast, and accurate capillary zone electrophoresis method has been developed for the determination of ciprofloxacin and ofloxacin. This method uses liquid–liquid extraction. Therefore, it is characterized by a very simple procedure of sample preparation but at the same time satisfactory precision and accuracy. The extraction process of the same urine sample was repeated three times. The extraction protocol was performed each time for 15 min with 1 mL of dichloromethane and chloroform mixture in a 3:1 volume ratio. A 0.1 mol/L phosphate-borate buffer (pH 8.40) was selected as the background electrolyte. UV detection was performed at 288 nm. The separation was carried out at a voltage of 16 kV, at a temperature of 25 °C. Experimentally evaluated LOQ values for ciprofloxacin and ofloxacin were 0.2 nmol/mL urine and 0.05 nmol/mL urine, respectively. For both analytes the calibration curves exhibited linearity over the entire tested concentration range of 1–6 nmol/mL urine. The precision of the method did not exceed 15%, and the recovery was in the range of 85–115%. The developed and validated procedure was applied to analyze human urine for the content of ciprofloxacin and ofloxacin.

Mn-DOPPED ZnS QUANTUM DOTS AS SENSITIVE SENSOR FOR DETERMINATION OF CIPROFLOXACIN IN PHARMACEUTICAL AND BIOLOGICAL SAMPLES

A simple and fast spectrofluorimetric method for determination of ciprofloxacin based on its quenching effect on the fluorescence intensity of colloidal water ­soluble TGA ­caped, Mn doped ZnS quantum dots (QDs) has been described. The QDs having characteristic fluorescence spectra with maximum excitation at 315 nm followed by an emission peak at 632 nm were characterized using Energy Dispersive X-Ray and X-ray Diffraction techniques. The effect of various parameters such as concentration of QDs, time, pH, common excipients and metal ions on the quenching phenomenon was investigated. Fluorescence quenching was found to be maximum with 10 µg mL­-1 of QDs at pH 8 and fluorescence intensity was observed to be constant upto 45 min. The Stern­-Volmer calibration plot of F0/F as a function of ciprofloxacin concentration was found to be linear in the range of 0.5-10 µg mL­-1 with r² = 0.993. Under optimal experimental conditions the method was found to be interference free. The percent relative standard deviation of the proposed method calculated against method blank was found to be 1.10%. The limit of detection (LOD) and the limit of quantitation (LOQ) for Cf (signal to noise ratio 3:1 for LOD and 10:1 for LOQ) were calculated to be 0.15 and 0.50 μg mL-1 respectively. Average percent recoveries (±SD) obtained for spiked commercial formulations; ciprol and ciproquine, and serum and urine samples were found to be in the range of 92.2±1.8% to 99.5±1.5%, 90.5±1.2% to 96.7±1.4% and 94.0±1.2% to 98.5±1.4% respectively. The data evidently prove the potential of the proposed sensor QDs in biological analysis.

A reliable chromatographic method for the simultaneous determination of ciprofloxacin and moxifloxacin in human serum

Purpose: To develop and validate a simple chromatographic method for the analysis of ciprofloxacin and moxifloxacin in human serum.Methods: After protein precipitation had been performed, high performance liquid chromatography (HPLC) with UV detection was utilized for the analysis of ciprofloxacin and moxifloxacin in human serum. Analytical column Zorbax SB-C18 (150 mm x 4.6 mm i.d., particle size 3.5 μm) was used as a stationary phase. Chromatographic separation was realized with the mobile phase 0.1% trifluoroacetic acid in water for chromatography - methanol (66:34, v/v), at the flow rate of 1 mL/min, temperature of 35 oC and detection at 280 nm. The method validation was performed according to the guidelines of the European Medicines Agency (EMA).Results: The chromatographic run time was about 12 minutes and no interference was observed. For ciprofloxacin, the method was linear over a concentration range of 0.5-50 μg/mL, with a correlation coefficient of 0.9874. For moxifloxacin, the method was linear over a concentration range of 0.5-50 μg/mL, with a correlation coefficient of 0.9946. Since relative standard deviation (RSD) and relative recovery values were within acceptable limits according to EMA guidelines, good intra-day precision, inter-day precision, as well as the accuracy of the method, were observed.Conclusion: A simple and reliable HPLC-UV method has been developed and validated for the simultaneous determination of ciprofloxacin and moxifloxacin in human serum. The method can be applied for therapeutic drug monitoring but also and pharmacokinetic studies of ciprofloxacin and moxifloxacin.
 Keywords: Human serum, Ciprofloxacin, Moxifloxacin, Protein precipitation, HPLC, UV detection, Method validation

A Simple, Cost‐effective, and Environmentally Friendly Method for Determination of Ciprofloxacin in Drugs and Urine Samples Based on Electrogenerated Chemiluminescence

AbstractCiprofloxacin is an antibiotic that belongs to the class of drugs known as quinolones and it is frequently used to treat a variety of bacterial infections. The present work aims the development of a simple, cost‐effective, and environmentally friendly method for the determination of ciprofloxacin in drugs and artificial urine samples due to the high importance of this antibiotic for the human health. The proposed method is based on the electrogenerated chemiluminescence (ECL) resulting from the reaction between the ciprofloxacin and the tris(2,2′‐bipyridyl)ruthenium(II) complex. This method exploits a screen‐printed carbon electrode positioned in an ECL cell with capacity to 50 μL of electrolytic solution. The ECL intensity was monitored with the aid of a photodiode. The ECL signal was simultaneously registered to the voltammetric measurements. Under optimized experimental conditions, the ECL method presented a linear response range for ciprofloxacin between 0.5 and 500 μmol L−1 (or 0.0005 and 0.5 mmol L−1). The proposed method presented a detection limit of 0.5 μmol L−1 and it was successfully applied for the ciprofloxacin determination in drugs and artificial urine samples, with good accuracy and precision.

Chemometrics - Assisted UV Spectrophotometric Method for Determination of Ciprofloxacin and Ornidazole in Pharmaceutical Formulation

Chemometrics - Assisted UV Spectrophotometric Method for Determination of Ciprofloxacin and Ornidazole in Pharmaceutical Formulation

New Analytical Method Development and Validation of Ciprofloxacin and Ornidazole in Human Plasma by High Performance Thin Layer Chromatography

Objective: The objective of the method was to develop a simple, rapid, sensitive, selective and economic high performance thin layer chromatographic method for simultaneous determination of ciprofloxacin and ornidazole in human plasma by using tinidazole as an internal standard. Method: The plasma sample was extracted using methanol: formic acid (5.5:0.5 v/v) and known amount of extract was spotted on precoated silica gel 60 F 254 plates using Camag Linomat V auto sampler. A concentration range from 100–700 ng/spot for both drugs was used for calibration curve. The percent recoveries of Ciprofloxacin and ornidazole were found to be 81.02 to 86.26 and 79.73 to 82.16 respectively. The mobile phase used consists of chloroform: methanol: triethylamine (9.0: 0.8: 0.4 v/v/v). Densitometric analysis was carried at wavelength 291 nm. Result: The R f values for ciprofloxacin, ornidazole and tinidazole were found to be 0.18 ± 0.057, 0.49 ± 0.0.0057 and 0.75 ± 0.0054 respectively. The stability of ciprofloxacin and ornidazole in plasma were confirmed during three freeze-thaw cycles (-20oC), on bench during 12 h and post preparative stability study. The proposed method was validated statistically by performing recovery study for determination of ciprofloxacin and ornidazole in human plasma. Conclusion: The proposed method was found to be a simple, rapid, sensitive, selective and economic high performance thin layer chromatographic method for simultaneous determination of ciprofloxacin and ornidazole in human plasma In future this method can be used for clinical and pharmacokinetic studies. Key words: Ciprofloxacin, Ornidazole, HPTLC, Human plasma, Liquidliquid extraction.

A simple and sensitive high-performance liquid chromatography method for determination of ciprofloxacin in bioavailability studies of conventional and gastroretentive prolonged-release formulations.

Background:A very simple, sensitive, and accurate high-performance liquid chromatography (HPLC) method with ultraviolet detector was developed and applied to determine ciprofloxacin in human plasma following administration of a gastroretentive formulation developed in our laboratory.Materials and Methods:HPLC analysis was performed on a C18 μ-Bondapack column (250 mm × 3.9 mm) using acetonitrile: potassium dihydrogen phosphate solution 0.1 M (20:80, v/v, pH 3) at a flow rate of 1.5 ml/min and eluate was monitored at 276 nm. After addition of phenacetin as internal standard, plasma samples were treated with 0.1 M phosphate buffer (pH: 7) and followed by extraction with dichloromethane. The method was validated for linearity, precision, accuracy, limit of quantitation (LOQ), robustness, stability, and applied in bioavailability studies of our developed gastroretentive formulation in healthy volunteers.Results:The calibration curves were linear over the concentration range 0.025–4 μg/ml with the detection limit of 15 ng/ml. Accuracy % were within 93–115 and the coefficient of variance % ranged from 0.20 to 12.8. The very low LOQ (25 ng/ml) allowed avoiding fluorometric detection which is more expensive and is not available in all laboratories. Ciprofloxacin was stable in samples with no evidence of degradation during 3 freeze-thaw cycles and 3 months storage at –70°C.Conclusion:This validated HPLC method was successfully used for the determination of ciprofloxacin in human plasma following oral administration of controlled release formulation, conventional immediate-release tablets and when administered concomitantly with divalent and trivalent cations such as aluminum-, magnesium-, or calcium-containing products under which the bioavailability of ciprofloxacin is significantly reduced.

Separation and characterization of ciprofloxacin, difloxacin, lomefloxacin, norfloxacin, and ofloxacin oxidation products under potassium permanganate treatment in acidic medium by UPLC-MS/MS

A simple, sensitive and reproducible ultra-performance liquid chromatography method for determination of ciprofloxacin, difloxacin, lomefloxacin, norfloxacin and ofloxacin oxidation stability under permanganate treatment in acidic conditions at pH from 3.0 to 6.0, was developed. Chromatographic separations were carried out using the Acquity UPLC BEH C18 column; (2.1×100mm, 1.7μm particle size). The column was maintained at 40°C, and eluted under isocratic conditions using 83% of eluent A and 17% of eluent B over 6.5min, at a flow rate of 0.3mLmin−1. Eluent A: water/formic acid (0.1v/v%); eluent B: acetonitrile/formic acid (0.1v/v%). An oxidation process followed kinetic of the second order reaction and depended upon solution acidity.Oxidation of fluoroquinolones proceeded at piperazine moiety yielding respective hydroxy and oxo analogs, and remaining the quinolone fragment intact. Structures of products formed were assigned on a basis of UPLC/MS/MS fragmentation pathways.

Flow-injection enhanced chemiluminescence method for determination of ciprofloxacin in pharmaceutical preparations and biological fluids

A novel rapid and sensitive analytical method, enhanced chemiluminescence with flow-injection sampling, is described for determination of ciprofloxacin. The method is based on the chemiluminescence reaction of the potassium permanganate-sodium thiosulfate-ciprofloxacin system. An enhanced chemiluminescence reaction was developed, and optimum conditions for CL emission were investigated. The chemiluminescence intensity was linearly dependent on ciprofloxacin concentration in the range 1.0 x 10(-8)-1.0 x 10(-5) g mL(-1). The detection limit was 4 x 10(-9) g mL(-1). The relative standard deviation was 1.8% for eleven measurements of 2.0 x 10(-7) g mL(-1) ciprofloxacin standard solution. The new method enables simple, sensitive, and rapid determination of ciprofloxacin and has been successfully used for determination of ciprofloxacin in biological fluids and in ciprofloxacin hydrochloride tablet and injection.

Solid-phase UV spectrophotometric method for determination of ciprofloxacin

A simple and inexpensive method for the determination of ciprofloxacin has been developed using solid-phase spectrophotometry. The intrinsic absorbance of ciprofloxacin fixed on a dextran-type cation-exchange resin, Sephadex SP C-25, was measured directly at 277 and 380 nm after packing the gel beads in a 1-mm cell. Using a sample volume of 10 ml, the calibration graph was linear over the range 0.05–0.3 μg ml −1 with a R.S.D. of 1.11% ( n=8). The sensitivity obtained is 40 times higher than that of the corresponding solution method. The method was applied to the determination of ciprofloxacin in pharmaceutical preparations and was validated by standard addition.

Simple High-Performance Liquid Chromatographic Method for Determination of Ciprofloxacin in Human Plasma

Arapid, simple and sensitive high-performance liquid chromatography method was developed for determination of ciprofloxacin in plasma by means of ultraviolet detection. Ofloxacin was used as an internal standard and separation carried on a Novapak C18 column using a mobile phase of 0.01 M phosphate buffer (pH =2.6): methanol (82:18 v/v). Extraction of drug was performed from plasma by liquid-liquid extraction and the average recovery was 78.2% The assay is precise, with inter-assay coefficient of variation of 6.70 % at 0.25-8 kg/ml (n=3). Using UVdetection at 277 nm the detection limit for ciprofloxacin was 20 ng/ml of plasma and the mean extraction recovery was 78.2 %. Short elution time, using UVdetector and usage of ofloxacin as internal standard are advantages of this method

Optimisation of a dialytic set-up for liquid chromatography: automated separation and preconcentration of ciprofloxacin

Continuous-flow and static dialysis coupled on-line to liquid chromatography was evaluated and an automated method for determination of ciprofloxacin in biological samples developed. A trace enrichment column packed with C 18 material and coupled with a continuous dialysis and reversed-phase HPLC system with fluorescence detection enabled determination of ciprofloxacin in human blood serum at the 0.1-nmol/l level. The amount of analyte preconcentrated and loaded on the HPLC system was linearly proportional to the concentration in the dialysed sample over more than 4 orders of magnitude (up to 1·10 −6 M). Data for linearity, repeatability and detectability for each particular set-up are given. The trace enrichment step eliminates band broadening caused by solvents different from those of the eluent and affecting retention of ciprofloxacin on the analytical column (increase in k′) due to the on-column change of eluent composition. In analysis of human serum samples phthalates leached from plastic materials may interfere due to coelution with the analyte.

Simultaneous high-performance liquid chromatographic determination of ciprofloxacin, fenbufen and felbinac in rat plasma

Ciprofloxacin (CPFX) is a new quinolone agent with potent, broad antibacterial activity. It is well absorbed and widely distributed into various body tissues and fluids when given orally [1,2]. Recently, it was reported that severe convulsion was induced in some patients who were given new quinolone antibacterial agents and non-steroidal anti-inflammatory drugs, including fenbufen (FNB) [3,4], which was later reported to potentiate the convulsant activity of various quinolones in mice [5]. FNB is readily biotransformed into 4-biphenylacetic acid (felbinac, FLB), which possesses anti-inflammatory activity [6-81. Therefore, in order to investigate possible pharmacokinetic interaction between these drugs, it is necessary to develop a simple, sensitive, selective and simultaneous assay method for the quinolone, FNB and FLB in biological fluids. We have already developed high-performance liquid chromatographic (HPLC) methods for simultaneous determination of quinolone involving ofloxatin, enoxacin or norfloxacin with FNB and FLB [9-l 11, and examined the effects of FNB and FLB on the pharmacokinetics of these three quinolones [12-141. However, no investigation has been carried out on the pharmacokinetic interaction of the newer quinolone, CPFX, with FNB and FLB. This paper describes a novel analytical method for the simultaneous determination of CPFX, FNB and FLB in rat plasma.

High-performance liquid chromatographic method for determination of ciprofloxacin in biological fluids

A simple and precise high-performance liquid chromatographic procedure has been developed for the determination in biological fluids of ciprofloxacin, a new, with extended antibacterial spectrum, quinoline carboxylic acid. The work-up procedure involves a chemical extraction step followed by isocratic chromatography on a reversed-phase analytical column, with ultraviolet detection. The detection limit for blood levels is 10 ng/ml. The calibration curve is linear from this detection limit to 10 μg/ml. The statistical analysis of the correlation made between this assay and an agar diffusion procedure during a pharmacokinetic study suggests the existence of one or more active metabolites which could be mainly excreted in the bile.

Analysis of ciprofloxacin and gentamicin diffusion in Proteus mirabilis O18 biofilm by laser interferometry method.

Laser interferometry is a measurement technique used in physical sciences, with a potential for new applications in microbiology. Our previously studies, focused on the quantitative analysis of antibiotics diffusion through membranes or their releasing from gel structure, indicate that this method might be useful in analysis of substances diffusion across the bacterial biofilms. As antibiotic - biofilm interaction model, we tested above method for determination of ciprofloxacin or gentamicin diffusion through Proteus mirabilis O18 biofilm. Laser interferometry analysis of antibiotics diffusion showed that the amount of ciprofloxacin transported through mature biofilm is 1.9 times higher than gentamicin. It was correlated with lower level of gentamicin in compare to the level of ciprofloxacin in biofilm, which amounts were predicted in biofilm during diffusion process by laser interferometry method. We suggest that the analysis of antibiotic diffusion in biofilm might by helpful in evaluation of effectiveness of antibacterial agents.