A simple reversed phase HPLC method was developed and validated for the simultaneous determination of sparfloxacin (SPFX), diclofenac sodium, meloxicam, ibuprofen, flurbiprofen, naproxen and mefenemic acid in a relati...A simple reversed phase HPLC method was developed and validated for the simultaneous determination of sparfloxacin (SPFX), diclofenac sodium, meloxicam, ibuprofen, flurbiprofen, naproxen and mefenemic acid in a relatively short time with high linearity in bulk material, pharmaceutical formulations and human serum. Purospher STAR C18 (250 × 4.6 mm, 5 μm) column was utilized with mobile phase, methanol and water (90:10, v/v pH 2.70 adjusted by phosphoric acid), was delivered at a flow rate of 1.5 mL.min–1. Eluent was monitored using UV detector at 240 nm. The proposed method is specific, accurate (98.42% - 102.75%), precise (intra-day and inter-day variation 0.011% - 1.85%) and linear (R2 > 0.999) with in the desired range 0.15 - 40 μg.mL–1 and the detection and quantification limit was 1.19E+08 – 0.150 μg.mL–1 and 3.62E+08 – 0.4574 μg.mL–1 respectively for SPFX and NSAIDs. The analysis of variance (ANOVA) and student’s t-test were applied to verify the results. The anticipated method is applicable to routine analysis of SPFX and NSAIDs in pharmaceutical formulations as well as in human serum samples. It has also applied on interaction of SPFX with NSAIDs.展开更多
Plasma quinolone concentrations are not routinely measured in clinical practice.However,in order to optimize quinolone treatment,monitoring of plasma concentrations could sometimes be useful particularly in critically...Plasma quinolone concentrations are not routinely measured in clinical practice.However,in order to optimize quinolone treatment,monitoring of plasma concentrations could sometimes be useful particularly in critically ill patients.In this study,anti-sparfloxacin antibody was obtained by immunizing rabbits with sparfloxacin conjugated with bovine serum albumin using isobutyl chloroformate method.After the assay procedure was optimized,the standard curve of sparfloxacin was established.The practical measuring range of the competitive ELISA extended from 5 ng/mL to 2 mg/mL.The recovery rates and coefficients of variation for rat plasma,urine and tissues were 87.7-106.2% and 4.8-15.3%,respectively.To demonstrate the potential of the ELISA,a preliminary pharmacokinetics and tissue distribution study of sparfloxacin in rats and quantitative analysis of sparfloxacin in several pharmaceuticals were performed and compared with high-performance liquid chromatography(HPLC).The experimental data indicated that the proposed method would be a valuable tool in therapeutic drug monitoring(TDM) for sparfloxacin.展开更多
Sparfloxacin can be oxidized by nitrous acid, then react with hydroiodic acid to form a fluorescent derivative. Based on this, a reversed-phase high performance liquid chromatographic pre-column derivatization new met...Sparfloxacin can be oxidized by nitrous acid, then react with hydroiodic acid to form a fluorescent derivative. Based on this, a reversed-phase high performance liquid chromatographic pre-column derivatization new method is described for the determination of sparfloxacin in human urine. The linear range is 0.05 mg/L to 4.0 mg/L, the recoveries are 91.5%similar to 95.7% and the RSD is 1.2%similar to4.2%. The results showed that this method is suitable for the determination of sparfloxacin in human urine.展开更多
In acid medium, sparfloxacin is oxidized by nitrous acid, then reacts with hydrobromic acid to form a new fluorescence substance, which can emit the strong fluorescence. which is 151 fold more than that of sparfloxaci...In acid medium, sparfloxacin is oxidized by nitrous acid, then reacts with hydrobromic acid to form a new fluorescence substance, which can emit the strong fluorescence. which is 151 fold more than that of sparfloxacin itself. By this, a new sensitive method for the determination of sparfloxacin in human urine by derivative-synchronous fluorescence is presented with good results.展开更多
The binding of sparfloxacin and bovine serum albumin(BSA) in aqueous solution was studied by means of fluorescence and absorbance spectra, and the interactions influenced by Fe 3+ and Cu 2+ were explored. Based ...The binding of sparfloxacin and bovine serum albumin(BSA) in aqueous solution was studied by means of fluorescence and absorbance spectra, and the interactions influenced by Fe 3+ and Cu 2+ were explored. Based on the Scatchard′s site binding model and fluorescence quenching, practical formulas for a small molecule ligand attaching to a bio-macromolecule are proposed. The binding parameters were measured according to the suggested models, and the binding distance, the transfer efficiency of energy between sparfloxacin and BSA were obtained in view of the Frster theory of non-radiation energy transfer. The effect of sparfloxacin on the conformation of BSA was analyzed by means of synchronous fluorescence spectroscopy.展开更多
Based on the self-ordered ring(SOR) fluorescence microscopic imaging technique on a hydrophobic glass slide with Zn 2+ and cetyltrimethyl ammonium bromide(CTMAB) as sensitizer,and poly(vinyl alcohol)-124(PVA-124) and ...Based on the self-ordered ring(SOR) fluorescence microscopic imaging technique on a hydrophobic glass slide with Zn 2+ and cetyltrimethyl ammonium bromide(CTMAB) as sensitizer,and poly(vinyl alcohol)-124(PVA-124) and NH 3-NH 4 Cl(pH 10.00) as the medium,a method has been developed for determining sparfloxacin(SPFX) concentrations in chicken serum and residues in chicken tissues and manures.When the droplet volume was 0.20 μ L,SPFX was determined in the range of 1.38×10-13 ~2.03×10-12 mol.ring-1(or 6.90×10-7 ~1.02×10-5 mol.L-1),and the limit of detection(LOD) was 14fmol.ring-1(or 6.90× 10-8 mol.L-1).The recoveries of SPFX at all different spiked levels are in the range of 90.74%~106.61% when the methanol or acetonitrile were used as extracting agent,respectively,and the relative standard deviations(RSDs) are less than 3.0%.This study expands the applied fields of SOR technique in drug concentrations and residues determination.展开更多
文摘A simple reversed phase HPLC method was developed and validated for the simultaneous determination of sparfloxacin (SPFX), diclofenac sodium, meloxicam, ibuprofen, flurbiprofen, naproxen and mefenemic acid in a relatively short time with high linearity in bulk material, pharmaceutical formulations and human serum. Purospher STAR C18 (250 × 4.6 mm, 5 μm) column was utilized with mobile phase, methanol and water (90:10, v/v pH 2.70 adjusted by phosphoric acid), was delivered at a flow rate of 1.5 mL.min–1. Eluent was monitored using UV detector at 240 nm. The proposed method is specific, accurate (98.42% - 102.75%), precise (intra-day and inter-day variation 0.011% - 1.85%) and linear (R2 > 0.999) with in the desired range 0.15 - 40 μg.mL–1 and the detection and quantification limit was 1.19E+08 – 0.150 μg.mL–1 and 3.62E+08 – 0.4574 μg.mL–1 respectively for SPFX and NSAIDs. The analysis of variance (ANOVA) and student’s t-test were applied to verify the results. The anticipated method is applicable to routine analysis of SPFX and NSAIDs in pharmaceutical formulations as well as in human serum samples. It has also applied on interaction of SPFX with NSAIDs.
文摘Plasma quinolone concentrations are not routinely measured in clinical practice.However,in order to optimize quinolone treatment,monitoring of plasma concentrations could sometimes be useful particularly in critically ill patients.In this study,anti-sparfloxacin antibody was obtained by immunizing rabbits with sparfloxacin conjugated with bovine serum albumin using isobutyl chloroformate method.After the assay procedure was optimized,the standard curve of sparfloxacin was established.The practical measuring range of the competitive ELISA extended from 5 ng/mL to 2 mg/mL.The recovery rates and coefficients of variation for rat plasma,urine and tissues were 87.7-106.2% and 4.8-15.3%,respectively.To demonstrate the potential of the ELISA,a preliminary pharmacokinetics and tissue distribution study of sparfloxacin in rats and quantitative analysis of sparfloxacin in several pharmaceuticals were performed and compared with high-performance liquid chromatography(HPLC).The experimental data indicated that the proposed method would be a valuable tool in therapeutic drug monitoring(TDM) for sparfloxacin.
文摘Sparfloxacin can be oxidized by nitrous acid, then react with hydroiodic acid to form a fluorescent derivative. Based on this, a reversed-phase high performance liquid chromatographic pre-column derivatization new method is described for the determination of sparfloxacin in human urine. The linear range is 0.05 mg/L to 4.0 mg/L, the recoveries are 91.5%similar to 95.7% and the RSD is 1.2%similar to4.2%. The results showed that this method is suitable for the determination of sparfloxacin in human urine.
文摘In acid medium, sparfloxacin is oxidized by nitrous acid, then reacts with hydrobromic acid to form a new fluorescence substance, which can emit the strong fluorescence. which is 151 fold more than that of sparfloxacin itself. By this, a new sensitive method for the determination of sparfloxacin in human urine by derivative-synchronous fluorescence is presented with good results.
文摘The binding of sparfloxacin and bovine serum albumin(BSA) in aqueous solution was studied by means of fluorescence and absorbance spectra, and the interactions influenced by Fe 3+ and Cu 2+ were explored. Based on the Scatchard′s site binding model and fluorescence quenching, practical formulas for a small molecule ligand attaching to a bio-macromolecule are proposed. The binding parameters were measured according to the suggested models, and the binding distance, the transfer efficiency of energy between sparfloxacin and BSA were obtained in view of the Frster theory of non-radiation energy transfer. The effect of sparfloxacin on the conformation of BSA was analyzed by means of synchronous fluorescence spectroscopy.
基金The National Nature Science Foundation of China(Grant Nos.21177163)111 Project B08044+2 种基金the Fundamental Research Funds for the Central Universities(0910KYZY45)"985 Project"of Minzu University of China(MUC 98507-08)"211 Project"of Minzu University of China(MUC 02121103)
文摘Based on the self-ordered ring(SOR) fluorescence microscopic imaging technique on a hydrophobic glass slide with Zn 2+ and cetyltrimethyl ammonium bromide(CTMAB) as sensitizer,and poly(vinyl alcohol)-124(PVA-124) and NH 3-NH 4 Cl(pH 10.00) as the medium,a method has been developed for determining sparfloxacin(SPFX) concentrations in chicken serum and residues in chicken tissues and manures.When the droplet volume was 0.20 μ L,SPFX was determined in the range of 1.38×10-13 ~2.03×10-12 mol.ring-1(or 6.90×10-7 ~1.02×10-5 mol.L-1),and the limit of detection(LOD) was 14fmol.ring-1(or 6.90× 10-8 mol.L-1).The recoveries of SPFX at all different spiked levels are in the range of 90.74%~106.61% when the methanol or acetonitrile were used as extracting agent,respectively,and the relative standard deviations(RSDs) are less than 3.0%.This study expands the applied fields of SOR technique in drug concentrations and residues determination.