环丙沙星与环糊精超分子体系的研究

利用荧光光谱法研究了环丙沙星与母体β-环糊精(β-CD)及其2种修饰衍生物羟丙基-β-环糊精(Hp-β-CD)、甲基-β-环糊精(Me-β-CD)形成的超分子体系,同时测定了3种超分子体系的猝灭常数和热力学参数.结果表明:环丙沙星与3种环糊精之间常温下均形成稳定的包合物;环丙沙星与3种环糊精包结过程中△G＜0和△H＜0,这说明环丙沙星与3种环糊精的包结能够自发进行而形成超分子体系,且反应为放热过程.通过对3种环糊精与环丙沙星的热力学数包结能力进行了比较,初步探讨了作用机理和影响包结能力大小的可能因素.     

鲁米诺-铁氰化钾化学发光体系对盐酸环丙沙星的测定

环丙沙星对NaOH介质中的鲁米诺-铁氰化钾的化学发光具有较强的增敏作用,据此建立了一种新的测定痕量环丙沙星药物的流动注射化学发光法。讨论了介质浓度、发光试剂浓度等因素的影响,在最佳实验条件下,环丙沙星的质量浓度在2.0×10-5~1.2×10-4g.L-1范围内与发光强度呈良好线性关系,检出限为1.2×10-6g.L-1,11次平行测定4.0×10-5g.L-1环丙沙星的相对标准偏差为3.2%。该方法已用于环丙沙星片剂的测定,所得结果与标示值相符。     

盐酸环丙沙星及其制剂含量测定方法的探讨

非水滴定法测定盐酸环丙沙星的含量时，需要预先加入冰乙酸和乙酸汞进行转化处理，两种试剂的加入顺序对盐酸环丙沙星的溶解速度影响较大，先加入乙酸汞时，盐酸环丙沙星溶解较快。用高效液相色谱法测定盐酸环丙沙星片及盐酸环丙沙星胶囊的含量时，如果以水作溶剂，测定值明显偏低，宜改用0.l mol／L盐酸溶液作溶剂。     

Simultaneous determination of trimethoprim,enrofloxacin, and ciprofloxacin in blood serum of poultry

A method is proposed for the simultaneous determination of trimethoprim, enrofloxacin, and ciprofloxacin in blood serum of poultry using HPLC. Samples were prepared using protein precipitation. The chromatographic separation of substances was attained on a C18 column using a mixture of a 50 mM acetate buffer solution (pH 3.0) with acetonitrile (86: 14) as a mobile phase. Detection was performed at 278 nm. Linearity was observed in the concentration range 50–5000 ng/mL for trimethoprim and 10–5000 ng/mL for ciprofloxacin and enrofloxacin. Precision was ≤2.1% for enrofloxacin, ≤1.6% for ciprofloxacin, and ≤14% for trimethoprim. Accuracy was ≤10.2% for enrofloxacin, ≤9.9% for ciprofloxacin, and ≤11.9% for trimethoprim. The method was applied to pharmacokinetic studies of complex antibacterial drugs containing trimethoprim and enrofloxacin as active substances.     

环丙沙星在BTR缓冲液中的紫外光谱性质研究与应用

研究了不同缓冲溶液 ,不同pH介质中环丙沙星的紫外光谱性质 ,提出在BrittonRobinson(BTR)缓冲溶液中为紫外分光光度法测定环丙沙星的最佳条件 .在吸收波长 2 77nm处 ,测得其表观摩尔吸收系数为 2 .6 3× 10 4L/mol.cm ,浓度在 3.0～ 2 3.0mg/L范围内 ,吸收度与浓度符合比尔定律 ,该法成功用于药物制剂中环丙沙星含量的测定 ,结果满意     

Determination of enrofloxacin and its metabolite ciprofloxacin in goat milk by high-performance liquid chromatography with diode-array detection. Optimization and validation

A high-performance liquid chromatography-diode array detection method (HPLC-DAD) combined with liquid chromatography-mass spectrometry was developed for the determination of enrofloxacin and its metabolite ciprofloxacin in goat milk. The HPLC-DAD method validation was compliant with the "DG SANCO 1805/2000" European regulation. The residues were extracted from milk with phosphate buffer, purified on a C18 Speedisk cartridge SPE (Baker) and then analysed using HPLC-DAD set at 277 nm. The decision limit (CCa) calculated by spiking samples at 100 microg/kg with both analytes, taking into account the maximum residue limit (MRL) of 100 microg/kg established by the European Union for the sum of enrofloxacin and its metabolite ciprofloxacin in milk, was 105.3 microg/kg for enrofloxacin and 105.5 microg/kg for ciprofloxacin. The detection capability (CCbeta) was 110.7 and 110.9 microg/kg for enrofloxacin and ciprofloxacin, respectively. The mean recoveries of the method, calculated by spiking samples at 50, 100 and 150 microg/kg were 84% for enrofloxacin and 88% for ciprofloxacin. The limit of quantification was 20 microg/kg for both analytes. The HPLC-DAD validated method was successfully applied for the first time in goats milk, and proved to be suitable for the sensitive and accurate quantification and confirmation analysis of enrofloxacin and ciprofloxacin for regulatory purposes.     

Determination of ciprofloxacin in human urine and serum samples by solid-phase spectrofluorimetry

A method for the determination of trace amounts of ciprofloxacin has been developed, based on solid-phase spectrofluorimetry. The relative fluorescence intensity of ciprofloxacin fixed on Sephadex SP C-25 gel was measured directly after packing the gel beads in a 1-mm silica cell, using a solid-phase attachment. The wavelengths of excitation and emission were 272 and 448 nm, respectively. Using a sample volume of 1000 ml, the linear concentration range of application was 0.3-10.0 ng.ml(-1) of ciprofloxacin, with a R.S.D. of 1.2% (for a level of 4.0 ng.ml(-1)) and a detection limit of 0.1 ng.ml(-1). The method was applied to the determination of ciprofloxacin in human urine and serum samples. It was validated applying the standard addition methodology and using HPLC as a reference method. Recovery levels of the method reached 100% in all cases.     

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 1.0×10⁻⁸–1.0×10⁻⁵ g mL⁻¹. The detection limit was 4×10⁻⁹ g mL⁻¹. The relative standard deviation was 1.8% for eleven measurements of 2.0×10⁻⁷ 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.     

Crystal structure of ciprofloxacin hydrochloride 1.34-hydrate.

Ciprofloxacin belongs to a family of quinolone antibacterial agents. The crystal structure of ciprofloxacin hydrochloride 1,34-hydrate was determined. Most of the bond lengths and angles of the ciprofloxacin cation are very similar to those of ciprofloxacin hexahydrate, which appears in the zwitterionic form. The exceptions are the carbon-oxygen bond distances in the carboxylic group, since in the title compound this group is not deprotonated. Various inter- and intramolecular hydrogen bonds were found in the molecule and are described.     

Determination of ciprofloxacin with functionalized cadmium sulfide nanoparticles as a fluorescence probe

A novel assay of ciprofloxacin with a sensitivity at the microgram level is proposed based on the measurement of enhanced fluorescence intensity signals resulting from the interaction of functionalized nano-CdS with ciprofloxacin. The CdS nanoparticles was synthesized by thioacetamide (TAA) and cadmium nitrate (Cd(NO(3))(2)) in the alkaline solution. At pH 7.4, the fluorescence signals of functionalized nano-CdS were greatly enhanced by ciprofloxacin with the increase concentration of ciprofloxacin. Linear relationship can be established between the enhanced fluorescence intensity and ciprofloxacin concentration in the range of (1.25-8.75)x10(-4) mg mL(-1) ((3.77-26.4) x 10(-4)mmol L(-1)) or (8.75-1200) x 10(-4)mg mL(-1) ((26.4-3625) x 10(-4) mmol L(-1)). The limit of detection is 7.64 x 10(-6) mg mL(-1) (2.31 x 10(-5)mmol L(-1)). Based on this, a new direct quantitative determination method for ciprofloxacin in human serum samples without separation of foreign substances was established. The contents of ciprofloxacin in human serum samples were determined with recovery of 95-105% and relative standard deviation (R.S.D.) of 1.5-2.5%. This method was proved to be very sensitive, rapid, simple and tolerance of most interfering substances.     

LC Assay for Ciprofloxacin Hydrochloride Ophthalmic Solution

The objective of the current study was to develop and subsequently validate a simple, sensitive and precise reversed-phase LC method for the determination of ciprofloxacin hydrochloride in ophthalmic solution form. The chromatographic separation of ciprofloxacin hydrochloride was achieved on a Symmetry Waters C₁₈ column using UV detection at 275 nm. The optimized mobile phase consisted of 2.5% acetic acid solution: methanol:acetonitrile (70:15:15, v/v/v). The proposed method provided linear responses within the concentration range 1.0–6.0 μg mL⁻¹ for ciprofloxacin hydrochloride. Correlation coefficient (r) for the ciprofloxacin hydrochloride was 0.9994. The precision of the method was demonstrated using intra- and inter-day assay RSD% values which were less than 5% in all instances. No interference from any components of pharmaceutical dosage forms was observed.

     

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.     

Liquid Chromatographic Analysis of Ciprofloxacin and Ciprofloxacin Metabolites in Body Fluids

Abstract

An isocratic HPLC assay procedure for analysis of ciprofloxacin and three metabolites was developed. The procedure requires only dilution of bile, saliva, and urine samples prior to reverse-phase chromatography on a polystyrene-divinylbenzene (PSDVB) column; analysis of serum samples requires a cleanup step on a PSDVB cartridge prior to chromatography. The dependence of chromatographic efficiency on flow rate and temperature was investigated and the accuracy, precision, selectivity, and sensitivity of the procedure were evaluated. The developed procedure was also compared to a modified version of a published ciprofloxacin procedure that requires an octadecyl-silane (ODS) column for chromatographic separation. Similar efficiency, precision, and accuracy were observed with both procedures and both were used for analysis of clinical samples. However, the procedures were used for different purposes. The PSDVB procedure, because of more favorable column selectivity, was used to assay ciprofloxacin and its metabolites in bile, urine and saliva samples. The ODS procedure, because of a simpler serum preparation step, was used t o assay ciprofloxacin in serum samples.     

Flow injection spectrophotometric determination of the antibiotic ciprofloxacin in drug formulations.

A flow injection spectrophotometric method for the assay of ciprofloxacin was developed. The method was based on the chelation of iron(III) with the drug in 0.023 mol dm-3 sulfuric acid solution in a 72 cm long coil and the brown-red complex produced was monitored at 447 nm. The super modified simplex computer program was employed for the optimization of the system and chemical parameters with respect to throughput and sensitivity as a measure of system performance. A working range for ciprofloxacin determination of 50-500 ppm for a 110 mm3 sample size with an optimum of 250 samples per hour was achieved with a relative standard deviation of less than 0.92%. The method was successfully applied to the determination of ciprofloxacin in drug formulations.     

LC Assay for Ciprofloxacin Hydrochloride Ophthalmic Solution

The objective of the current study was to develop and subsequently validate a simple, sensitive and precise reversed-phase LC method for the determination of ciprofloxacin hydrochloride in ophthalmic solution form. The chromatographic separation of ciprofloxacin hydrochloride was achieved on a Symmetry Waters C₁₈ column using UV detection at 275 nm. The optimized mobile phase consisted of 2.5% acetic acid solution: methanol:acetonitrile (70:15:15, v/v/v). The proposed method provided linear responses within the concentration range 1.0–6.0 μg mL⁻¹ for ciprofloxacin hydrochloride. Correlation coefficient (r) for the ciprofloxacin hydrochloride was 0.9994. The precision of the method was demonstrated using intra- and inter-day assay RSD% values which were less than 5% in all instances. No interference from any components of pharmaceutical dosage forms was observed.     

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.     

碳糊电极阳极吸附伏安法测定环丙沙星

报道了用碳糊电极阳极吸附伏安法测定环丙沙星的新方法.在 0. 40mol/L的NH4Ac HAc(pH4. 30)缓冲液中,使用JP 303极谱分析仪,环丙沙星在碳糊电极 (CPE)上有一灵敏的吸附伏安氧化峰,峰电位为1. 12V(vs.SCE).该氧化峰的二阶导数峰电流与环丙沙星的浓度在 8. 0×10-9 ~8. 0×10-7 mol/L(富集 90s)范围内成良好的线性关系,相关系数为 0. 998 8,检出限为 4. 0×10-9 mol/L(S/N=3,富集 110s).探讨了环丙沙星在碳糊电极上的伏安性质和电极反应机理,并且成功应用于人体尿样中环丙沙星含量的测定.加入回收实验,回收率在95. 5%至 103. 9%之间.     

UPLC–MS/MS method validation of ciprofloxacin in human urine: Application to biodegradability study in microbial fuel cell

To enable the reliable quantification of ciprofloxacin in human urine, a sensitive and selective assay based on liquid chromatography–tandem mass spectrometry was developed. The chromatographic separation of the ciprofloxacin was carried out on a Zorbex Eclipse C₁₈ column using methanol and ammonium acetate as a mobile phase by the gradient elution method. The developed assay covered a wide range of concentrations (1.56–100 ng/mL) with a lower limit of detection of 0.76 ng/mL. Quantification was performed using the multiple reaction monitoring transitions 331.8/231 for ciprofloxacin and 362/318 for ofloxacin (internal standard). This assay was validated for linearity, accuracy, precision and recovery. The validated method was then applied to the biodegradability of ciprofloxacin (99%) from human urine in the microbial fuel cell.     

Critical points in the analysis of ciprofloxacin by high-performance liquid chromatography

Chromatographic analysis of the antibiotic compound ciprofloxacin on a C18 column proved to show some critical points. On a C18 column, ciprofloxacin analysis resulted in two peaks in the chromatogram. Effects of stock solution composition, mobile phase composition and type of stationary phase were investigated to understand the occurrence of both peaks. Esterification of the carboxylic group of ciprofloxacin was shown when methanol was used as stock solution solvent in acidic conditions. Secondly, a ciprofloxacin pK(a) value of 3.64 in water at position N-1 was found which could not fully explain the observation of the two peaks: mobile phase composition and type of stationary phase were also found to be important parameters with respect to the peak area ratio of both peaks.