环丙沙星在胶束体系中的荧光特性研究及应用

研究了环丙沙星在胶束体系中的荧光性质，发现十二烷基硫基酸对环丙沙星有较强的增敏作用。据此建立了胶束增敏荧光光谱法测定痕量环丙沙星的新方法，经样品测定，其线性范围为0．033－0．60μg.mL^-1，检出限为0．033μg.mL^-1，回收率为94．0％－98．1％相对标准偏差为1．5％－2．8％。     

氯化铯和氯化镧溶剂体系及四类新化合物的合成

研究了四元体系ＣｓＣｌ－ＬａＣｌ３－ＨＣｌ－Ｈ２Ｏ（２５℃、「ＨＣｌ」＝１３％（ｗｔ），２３％（ｗｔ）和ＣｓＣｌ－ＬａＣｌ３－ＨＡｃ－Ｈ２Ｏ（３０℃，「ＨＡｃ」＝４２％（ｗｔ））的平衡态的溶度数据，并给出制了相应的溶度图，共得到了ＣｓＣｌ．ＬａＣｌ３．４Ｈ２Ｏ、２ＣｓＣｌ．ＬａＣｌ３．２Ｈ２Ｏ和３ＣｓＣｌ．ＬａＣｌ３．３Ｈ２Ｏ３种化合物。对得到的新相进行了热分析，Ｘ射线粉末衍射及偏光性质的测定，依     

Oxidative transformation of ciprofloxacin by alkaline permanganate – A kinetic and mechanistic study

This spectroscopic study presents the kinetics and degradation pathways of oxidation of ciprofloxacin by permanganate in alkaline medium at constant ionic strength of 0.04 mol⁻³. Orders with respect to substrate, oxidant and alkali concentrations were determined. Effect of ionic strength and solvent polarity of the medium on the rate of the reaction was studied. The oxidation products were identified by LC-ESI-MS technique. Product characterization of ciprofloxacin reaction mixtures indicates the formation of three major products corresponding to m/z 263, 306, and 348 (corresponding to full or partial dealkylation of the piperazine ring). The piperazine moiety of ciprofloxacin is the predominant oxidative site to KMnO₄. Product analyses showed that oxidation by permanganate results in dealkylation at the piperazine moiety of ciprofloxacin, with the quinolone ring essentially intact. The reaction kinetics and product characterization point to a reaction mechanism that likely begins with formation of a complex between ciprofloxacin and the KMnO₄, followed by oxidation at the aromatic N1 atom of piperazine moiety to generate an anilinyl radical intermediate. The radical intermediates subsequently undergo N-dealkylation. Investigations of the reaction at different temperatures allowed the determination of the activation parameters with respect to the slow step of proposed mechanism. The proposed mechanism and the derived rate laws are consistent with the observed kinetics.     

In vitro study of experimental factors affecting the microdialysis results

The aim of the present study was to determine the influence of a series of experimental conditions (probe, perfusate flow rate and the method used to ascertain recovery) as well as the pharmacokinetic variables (concentration and time) on the estimation of the recovery coefficient of microdialysis probes. Two in vitro pharmacokinetic assays were also carried out to compare the results provided by microdialysis and those obtained with traditional sampling. The probes used were made in our laboratory and ciprofloxacin was used as a model compound. The results revealed that in all cases recovery was dependent on the probe and independent of time for a 80 min sampling time period. The effects of concentration on recovery depend on the flow rate; this was not statistically significant for a flow rate of 2 μl/min but an increase in flow rate to 6 μl/min transformed this parameter into a concentration-dependent variable. A decrease in recovery parallel to the increase in flow rate was found, with an exponential relationship between the two variables. Statistically significant differences were also found between the recovery values obtained for direct dialysis (18.44±1.61) and retrodialysis by loss of the analyte of interest (16.79±3.42). The values of the protein binding of ciprofloxacin as calculated by equilibrium dialysis and by microdialysis were similar. Characterization of the in vitro kinetic profile revealed no statistically significant differences for coefficients and exponents obtained by traditional sampling and microdialysis, although the confidence intervals of the curves were wider for microdialysis.     

UV/TiO2 photodegradation of metronidazole,ciprofloxacin and sulfamethoxazole in aqueous solution: An optimization and kinetic study

Emerging pharmaceutical ingredients (APIs) like sulfamethoxazole (SMX), metronidazole (MNZ) and ciprofloxacin (CIP) are biopersistent and toxic to the environment and public health. In this study, UV/TiO₂ photodegradation was applied in the degradation of SMX, MNZ and CIP individually and in a mixture. For a 5 mg/L SMX solution, about 97% of SMX was degraded within 360 min, which was reduced to 80% for 80 mg/L of SMX solution at the same TiO₂ dosage and photodegradation time. The maximum removals of MNZ and CIP as individual components were 100% and 89%, respectively at 600 min of photodegradation reaction time. For binary mixtures, the highest removal (100%) was achieved for MNZ and CIP ([MNZ] = [CIP] = 40 mg/L) mixture at 120 min whereas the degradations were 97% and 96% for SMX and MNZ, and SMX and CIP binary mixtures, respectively, even after 600 min of experimental time at the same concentrations. For tertiary mixture, the maximum degradation 99% was observed for (SMX = CIP] = 20 mg/L and [MNZ] = [40 mg/L) at 600 min. The observed reaction rate was 0.01085 min^?1 when SMX concentration was 5 mg/L, which decreased to 0.00501 min^?1 for SMX concentration of 80 mg/L, indicating decreasing of reaction rate at higher concentration. The results indicate that the UV/TiO₂ process is promising to apply for the treatment of pharmaceutical wastewaters.     

间接原子吸收法测定乳酸环丙沙星

研究了在弱酸性介质中，乳酸环丙沙星与雷氏盐定量生成缔合物的反应条件，以及通过原子吸收法测定沉淀中Cr的含量而间接测定乳酸环丙沙星含量的分析方法。线性范围在5－40mg/L，相对标准偏差为2．5％，回收率在98％－101％之间。     

Photocatalytic ozonation degradation of ciprofloxacin using ZnO nanoparticles immobilized on the surface of stones

Ciprofloxacin is used in the treatment of bacterial infections. Because ciprofloxacin is not effectively degraded by biological processes, advanced oxidation processes such as photocatalytic ozonation are applied to remove this antibiotic from wastewater. The aim of this study was to investigate photocatalytic ozonation for the removal of ciprofloxacin from aquatic environments and optimization of the effective parameters of the process. For this purpose, ZnO nanoparticles were synthesized using the thermal method and immobilized on the surface of stones. The structural properties of the nanoparticles were determined by XRD, TEM, Photoluminescence (PL) and SEM. Experiments were carried out in a Plexiglas reactor supported with the continuous injection of ozone. The effective parameters for removal efficiency were reaction time, initial concentration of ciprofloxacin, pH, photocatalyst concentration and reaction kinetics. The highest ciprofloxacin removal efficiency occurred at the following optimal conditions: pH of 7, reaction time of 30?min, photocatalyst concentration of 3?g/L and initial ciprofloxacin concentration of 10?mg/L. Removal efficiency of 96% was obtained under these conditions. Linear kinetic models showed that the process followed pseudo-first order and Langmuir-Hinshelwood kinetics. This process had a high removal efficiency and suitable for removal of ciprofloxacin from aquatic environments.GRAPHICAL ABSTRACT     

Use of the diphasic dialysis as a new extraction procedure in the determination of enrofloxacin and ciprofloxacin in egg

We have developed a new method for the analysis of the fluoroquinolones enrofloxacin and ciprofloxacin in eggs using a diphasic dialysis procedure as extraction and purification method. High pressure liquid chromatography-mass spectrometry (HPLC-MS) was used for the confirmatory determination of these compounds. The method was found to be linear between 10 and 800 ng g⁻¹ for enrofloxacin, and between 20 and 1600 ng g⁻¹ for ciprofloxacin. The recovery percentages were in the 70-104% range for enrofloxacin, and 55-97% for ciprofloxacin. The assay described was repeatable and reproducible with a limit of quantitation of 2 and 4 ng g⁻¹ for enrofloxacin and ciprofloxacin from egg, respectively.     

Flow-injection chemiluminescence determination of fluoroquinolones by enhancement of weak chemiluminescence from peroxynitrous acid

A flow-injection chemiluminescence (CL) method is described for the determination of fluoroquinolones including ciprofloxacin, norfloxacin and ofloxacin. The method is based on the enhancement by these compounds of the weak CL from peroxynitrous acid. The linear ranges are 1.0×10⁻⁷ to 1.0×10⁻⁵ mol l⁻¹ for ciprofloxacin and norfloxacin, and 3.0×10⁻⁷ to 3.0×10⁻⁵ mol l⁻¹ for ofloxacin, respectively. The detection limits (S/N=3) are 4.5×10⁻⁸ mol l⁻¹ ciprofloxacin, 5.9×10⁻⁸ mol l⁻¹ norfloxacin and 1.1×10⁻⁷ mol l⁻¹ ofloxacin, respectively. The proposed method was applied to the determination of fluoroquinolones in pharmaceutical preparations.     

Separation and determination of seven fluoroquinolones by pressurized capillary electrochromatography

In this paper, pressurized CEC was used for the separation and determination of seven fluoroquinolones (FQs). The effect of different experimental conditions, such as the concentration and pH of the buffer, the organic modifier concentration, the surfactant and ion-paring agents added to the electrolyte, and applied voltage were studied. All the seven FQs were baseline separated using mobile phase containing 27% v/v ACN, 5 mmol/L Na2HPO4 buffer (pH 4.0 adjusted using citric acid), 11 mmol/L SDS, and 0.01% TEA v/v at detection wavelength of 287 nm and at an applied voltage of -10 kV. The calibration curves were linear (r>0.9991) over a concentration range of 1.0-50.0 mg/L for norfloxacin (NFLX); 2.5-50.0 mg/L for fleroxacin (FLX), ciprofloxacin (CPFX), and lomefloxacin (LMX); and 5.0-50.0 mg/L for enoxacin (ENX), ofloxacin (OFLX), and gatifloxacin (GFLX). The detection limits (S/N = 3) for ENX, OFLX, FLX, NFLX, CPFX, LMX, and GFLX were 0.5, 0.8, 0.4, 0.2, 0.4, 0.5, and 1.0 mg/L, respectively. The method is simple, rapid, and reproducible. It was successfully applied to the analysis of fish muscle samples spiked with FQs. Mean recoveries ranged from 81.6 to 97.6%.