QUANTITATIVE ANALYSIS OF EIGHT CEPHALOSPORIN ANTIBIOTICS IN PHARMACEUTICAL PRODUCTS AND URINE BY CAPILLARY ZONE ELECTROPHORESIS
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Abstract:
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%.Keywords:
Cefixime
Cefadroxil
Ceftizoxime
Cefaclor
Quantitative Analysis
Cephalosporin Antibiotic
Absorbance
Cephradine
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An RP-HPLC method was founded,which could separate several cephalosporins under the same conditions simultaneously.Six drugs,ceftazidime,cephradine,cephalexin,cefotaxime,cefoperazone and cefazolin,were determined using ODS column,acetonitrile-HAC-NaAC buffer(pH=4.0) as mobile phase,and UV(λ_(max)=254?nm).These six drugs could be separated from each other in 15 minutes.The detect limits of these six drugs are all 0.20?μg·mL~(-1).The drug amounts in pharmaceutical formulations in human urine were determined by the proposed method.The results are satisfactory.The recovery rates of six drugs in human urine are all higher than 92.4%.It is proved that this method is simple,fast and sensitive.
Cephradine
Cefoperazone
Cefazolin
Cefadroxil
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A simple method for the separation and determination of cefadroxil, cefaclor, cefaloxin, cefradine and cefalotin etc. was completed on a C-16 silica stationary phase packed reversed-phase column with mobile phase of water/acetonitrile/phosphoric buffer (1 mL/min) in about. 17 min. The compounds were detected directly by ultraviolet detector at 270 nm. The linear range was 0.1-40 mg/L(r >= 0.9993) and the detection limits of cefadroxil, cefaclor, cefaloxin, cefradine and cefalotin were 9.7, 6.9, 5.6, 6.4 and 4.9 mu g/L, respectively. The method was applied successfully to the detection of cephalosporins in human urine and in bovine milk with the recovery of 96.5%-105% (when added sample was 2 mg/L).
Cefadroxil
Cefaclor
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A capillary zone electrophoresis (CZE) method was developed for the simultaneous determination of cefoperazone sodium and tazobactam sodium in the injectable powder of cefoperazone sodium and tazobactam sodium with hydrochlorothiazide as the internal standard. The operation was carried out on a quartz capillary (75 cm x 75 microm i. d. , 63 cm effective length). The electrophoretic conditions were as follows: 40 mmol/L borax solution as the back ground electrolyte (BGE), 12. 0 kV applied voltage, 220 nm as the detection wavelength; the sample solution was injected by hydraulic pressure for 10 s at the height of 10 cm. The cefoperazone and tazobactam showed good linear relationship in the ranges of 0.25-3.96 g/L and 0.062-0.99 g/L with the correlation coefficients of 0.999 5 and 0.999 6, respectively. The relative standard deviations of relative peak areas were less than 3%. The preparation was stable in 208 min. The recovery results met the methodology requirements. The method is simple, rapid, reproducible, and suitable to control the quality of cefoperazone sodium and tazobactam sodium injectable powder.
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A HPCE(high performance capillary electrophoresis) method for determination of cefuroxime sodium forinjection was established. A capillary column(75mm×60cm) was used with 30mmol/L borax (pH 9.2)as the electrophoreticbuffer, at the detection wavelength of 254nm. Ferulic acid was used as the internal standard. The calibration curve was linear inthe concentration range of 6～30mg/ml(r=0.9996). The average recovery was 98.9% with RSD of 1.82%.
Borax
Cefuroxime
Standard curve
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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
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This paper reported the research on the simultaneous separation and determination of six cephalosporins by RP-HPLC. Six cephalosporins are cefalcor, cefalexin, cefradine, cefadroxil, cefominox and cefoxitin. The analytical conditions for this method were as follows: a Hypersil ODS C18(200 mm x 4.6 mm i.d., 5 microns), detection wavelength: 254 nm; a mobile phase solution of 50 mmol/L monopotassium phosphate (pH 3.4)-acetonitrile (87.5:12.5) and DAD detector. The flow rate was 1.0 mL/min. The calibration curves of the six compounds were linear, the correlation coefficients were 0.9951 for cefominox, 0.9999 for the others, the range were 164 ng-16.4 micrograms for cefominox, 99 ng-9.934 micrograms for cefadroxil, 104 ng-10.358 micrograms for cefalcor, 122 ng-12.224 micrograms for cefalexin, 107 ng-10.702 micrograms for cefradine and 115 ng-11.506 micrograms for cefoxitin. The recovery rates were 103.5% for cefominox, 99.3% for cefadroxil, 101.4% for cefalcor, 101.5% for cefalexin, 98.7% for cefradine and 97.6% for cefoxitin. Six cephalosporins were all stable in 50 mmol/L monopotassium phosphate (pH 3.4-4.6). When preparations of these cephalosporins were determined, it is indicated there were no difference between the results by using this method and the pharmacopoeia methods. The total separation time of these cephalosporins was within fifteen minutes. This method is simple, sensitive, rapid and accurate.
Cefadroxil
Cefalexin
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A "high-performance" liquid-chromatographic technique involving a radial compression module is used for measuring chloramphenicol and five cephalosporin antibiotics: cefotaxime, cefoxitin, cephapirin, and cefamandol. Serum proteins are precipitated with acetonitrile solution containing 4'-nitroacetanilide as the internal standard. The drugs are eluted with a mobile phase of methanol/acetate buffer (30/70 by vol), pH 5.5. Absorbance of the cephalosporins is monitored at 254 nm. Standard curves are linear to at least 100 mg/L. The absorbance of chloramphenicol is monitored at 254 nm and 280 nm, and its standard curve is linear to at least 50 mg/L. The elution times for various other drugs were also determined, to check for potential interferents.
Absorbance
Standard curve
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A Validated RP-HPLC-UV Method for Simultaneous Estimation of Ceftriaxone and Sulbactum in Rat Plasma
A reverse phase - liquid chromatographic method with UV detection is developed for simultaneous estimation of ceftriaxone sodium and sulbactam sodium in rat plasma. A simple protein precipitation technique was employed for the extraction of drugs from blank plasma. Chromatographic separation of the two drugs was achieved on C18 column (250 mm X 4.6 mm, i.d, 5 μm) using a mobile phase consisting of 10mM potassium dihydrogen orthophosphate buffer (pH - 5) and aceto nitrile (90:10 % v/v). The developed liquid chromatographic method eluted both the drugs with a reasonable retention time, acceptable symmetric peak shape and good resolution. The developed bio - analytical method was linear, accurate, and precise over the co ncentration range of 20 - 150 μg mL - 1 for ceftriaxone and 10 - 75 μg mL - 1 for sulbactam. The developed method was successfully applied to monitor ceftriaxone and sulbactam sodium concentrations in rat plasma.
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A simple and fairly fast capillary zone electrophoresis method has been developed for the determination and separation of ceftriaxone, ceftizoxime, paracetamol, and diclofenac sodium in a mixture, in pharmaceutical formulations, and in blood serum. A 50 mM sodium tetraborate background electrolyte solution (pH 9.0) was found to be suitable for separation of all the drugs. An uncoated fused-silica capillary of a total length of 57 cm (effective length 50 cm) was used for separation. All the analytes were completely separated within 8.0 min at an applied voltage of 30 kV and detection was performed at 214 nm .Validation of the method was performed in terms of linearity, accuracy, precision and limit of detection, and quantification. The linearity of the calibration curves for paracetamol was 5-125 \mu g/mL, for ceftizoxime was 5-500 \mu g/mL, for diclofenac was 1-125 \mu g/mL, and for ceftriaxone was 10-1000 \mu g/mL, while LOD of the paracetamol, ceftizoxime, diclofenac, and ceftriaxone was found to be 1.0, 1.0, 0.5, and 5.0 \mu g/mL, respectively. The proposed method was applied for the determination of active ingredients in pharmaceutical formulations and active drugs in human blood serum. The recovery was found to be >= 99% with the relative standard deviation (RSD) Keywords: Capillary zone electrophoresis, paracetamol, ceftriaxone, ceftizoxime, diclofenac sodium
Ceftizoxime
Diclofenac Sodium
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A simple spectrophotometric method was developed for the determination of cefadroxil in pure bulk and in capsules forms. The method is based on a direct reaction between cefadroxil and sodium hydroxide (1 N). A product with λ max at 342 nm and molar absorptivity of 7.9x10 3 L mol -1 cm -1 is formed after heating cefadroxil with sodium hydroxide (1 N) for 30 minutes. The absorbance‐concentration plot was rectilinear over the range 5‐25 μg/mL with correlation coefficient values not less than 0.999. The detection limit (LOD) and quantification limit (LOQ) were 0.693 μg/mL and 2.31 μg/mL. The method was validated using the BP liquid chromatographic method for cefadroxil assay. The results obtained by the developed method for the capsules dosage form were statistically compared with those of the BP liquid chromatography method and evaluated at 95% confidence limits.
Cefadroxil
Sodium hydroxide
Absorbance
Molar absorptivity
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