Determination of Levofloxacin in Human Urine with Capillary Electrophoresis and Fluorescence Detector

In this study, we developed an analytical method for the enantioseparation of ofloxacin, using capillary electrophoresis with fluorescence detection. The optimum background electrolyte was obtained to be 60 mM hydroxylpropyl‐β‐cyclodextrin (HP‐β‐CD) in 50 mM phosphate buffer at pH 2.30. Under these conditions, the (+) and (‐) ofloxacin were completely separated, with the detection limit of 10 nM when the sample was prepared in deionized water. The linear ranges of levofloxacin in deionized water and untreated urine were 10^?7 to 5 × 10^?3 M with R² = 0.9989 and 5 × 10^?6to 5 × 10^?3 M with R² = 0.9943, respectively. We also applied this method to investigate the purity of a commercial drug. The results revealed that the ratio between (+)‐ofloxacin and (‐)‐ofloxacin (levofloxacin) was 99.9:0.1, and there is about 93 mg levofloxacin per tablet (200 mg). The concentration of levofloxacin in patient's urine was founded to be 7.9 × 10^?4M, and the ratio between the two optical isomers was 99.3:0.7.     

三维还原氧化石墨烯/β-环糊精复合物的合成及其电化学检测水中左氧氟沙星北大核心CSCD

成功构筑了β-环糊精修饰的三维还原氧化石墨烯复合材料(3D-rGO/β-CD),并对该复合材料进行扫描电子显微镜、傅里叶红外光谱、热重分析和拉曼光谱分析等一系列的表征,分析了其形貌和结构的特征。进一步将其修饰到玻碳电极(GCE)表面,构建了一种新型电化学传感器(3D-rGO/β-CD/GCE)。利用3D-rGO/β-CD/GCE电化学传感器,通过微分脉冲伏安法(DPV)对左氧氟沙星(LEV)进行了检测。其中,具有多孔结构的三维还原氧化石墨烯具有优异的导电性能、比表面积大、化学稳定性好等优良的性质,而修饰的β-环糊精能在其环形腔内与客体分子结合形成超分子包合物,进而可以对LEV进行有效识别。研究结果显示,在最优实验条件下,3D-rGO/β-CD/GCE对左氧氟沙星的检测具有较宽的线性范围(1~150μmol/L),且检测限可达0.33μmol/L,同时该修饰电极还表现出良好的选择性和稳定性。此外,成功将其应用于实际水样中LEV的检测,表明该传感器具有一定的应用潜力。     

无溶剂顶空气相色谱法测定盐酸左氧氟沙星残留溶剂

采用无溶剂-顶空-气相色谱直接测定盐酸左氧氟沙星中残留溶剂乙醇、甲苯、二甲基亚砜(DMSO)等.各残留溶剂的检出限分别在0.007-0.032 μg,6次测定的相对标准偏差RSD在1.84%-1.92%,加标回收在90.9%-110%.方法简便、快速、灵敏,可应用于其他药品中残留溶剂的分析.     

Rapid chiral separation and impurity determination of levofloxacin by ligand-exchange chromatography

A sensitive, simple, and accurate method for determination of levofloxacin and its (R)-enantiomer was developed to determine the chiral impurity of levofloxacin in Cravit Tablets material by ligand-exchange high performance liquid chromatography. The effects of different kinds of ligands, concentration of ligands in mobile phase, organic modifier, pH of mobile phase, and temperature on enantioseparation were investigated and evaluated. Chiral separation was performed on a conventional C₁₈ column, where the mobile phase consisted of a methanol-water solution (containing10 mmol L⁻¹l-leucine and 5 mmol L⁻¹ copper sulfate) (88:12, v/v) and its flow-rate was set at 1.0 mL min⁻¹. The conventional C₁₈ column offers baseline separation of two enantiomers with a resolution of 2.4 in less than 20 min. Thermodynamic data (ΔΔH and ΔΔS) obtained by Van’t Hoff plots revealed the chiral separation is an enthalpy-controlled process. The standard curves showed excellent linearity over the concentration range from 0.5 to 400 mg L⁻¹ for levofloxacin and its (R)-enantiomer. The linear correlation equations are: y = 1.33 × 10⁵x + 6297 (r = 0.9991) and y = 1.34 × 10⁵x + 3565 (r = 0.9997), respectively. The relative standard deviation (RSD) of the method was below 2.3% (n = 3).     

Thermodynamic and kinetic mechanism of phase transformation of levofloxacin hydrochloride

In this work, thermodynamic and kinetic factors that affect formation and phase transformation process of different solid forms of levofloxacin hydrochloride were investigated in detail. Dynamic vapor sorption experiments (DVS) and varying temperature-powder X-ray diffraction (VT-PXRD) experiments were carried out to study moisture-dependent stability, thermal stability as well as the transformation process between Form I and Form II. Critical water activities of levofloxacin hydrochloride were determined in temperature range of 5.0–45.0 °C. Raman spectroscopy was applied to in situ monitor the temperature-induced phase transformation and the hydration process of levofloxacin hydrochloride, and one possible mechanism consisting of multiple chemical equilibria was proposed to analyze the effect of thermodynamic and kinetic factors on the formation and transformation of different solid forms. Results show that the anhydrate, Form II would transform to the monohydrate, Form I more easily with the increasing water content. And the transition point moves toward higher water contents as the temperature increases. The results suggested that, except for thermodynamic factors, kinetic factors also play an essential role in controlling the solid forms of polymorphic compounds.     

左氧氟沙星选择性电极的制备及其性能研究

以左氧氟沙星与四苯硼酸根形成的缔合物为电活性物质,研制了一种左氧氟沙星PVC膜涂层玻璃电极,并对其响应性能进行了系统研究.实验表明,该电极的Nernst响应范围为5.0×10-3～2.0×10-5 moL/L,斜率为51.7 mV/pC,适用pH范围为3.0～4.5.该电极制作方法简单,响应迅速,重现性好,用于左氧氟沙星注射液和片剂的测定.     

Spectrophotometric Determination of Some Fluoroquinolone Antibacterials by Ion‐pair Complex Formation with Cobalt (II) Tetrathiocyanate

A new simple extractive spectrophotometric method has been developed for the determination of levofloxacin (I), norfloxacin (II), and ciprofloxacin (III) in pure form and tablets. The method is based on the formation of blue‐colored ion‐pair associates between the drugs and the inorganic complex, cobalt (II) thiocyanate, at pH 2.5. Those ion‐pair associates are readily extracted into an n‐butanol‐dichloromethane solvent mixture (3.5:6.5) and determined spectrophotometrically at 623 nm. The concentration range is 20–240 μg mL^?1 for the three studied drugs. The proposed method was successfully applied to determine these drugs in their tablet formulations, and the results are in good agreement with those obtained by the reference methods.     

The Interaction Between Levofloxacine Hydrochloride and DNA Mediated by Cu2+

Levofloxacin (LEV) is a fluoroquinolone antimicrobial agent. LEV also inhibits DNA synthesis and is bactericidal. The mechanisms of the interaction among LEV, DNA and Cu2+ are studied by fluorescence method. In the paper, the results show that LEV and Cu2+ can form binary complex, and also LEV and DNA can form complex mediated by Cu2+. The composition of the complex is determined. The affects to the reaction are also found.     

Antibiotic Detection in Urine Using Electrochemical Sensors Based on Vertically Aligned Carbon Nanotubes

A sensitive way to determine levofloxacin using a sensor based on vertical aligned carbon nanotubes is described. The morphology and the electrochemical performance of the electrodes were characterised by atomic force microscopy, cyclic voltammetry and square wave voltammetry. A scan‐rate study and electrochemical impedance spectroscopy showed that the levofloxacin oxidation product is adsorbed on the electrode surface. Differential pulse voltammetry in phosphate‐buffer solution allowed the development of a method to determine levofloxacin levels in the range of 1.0–10.0 µmol L^?1, with a detection limit of 75.2 nmol L^?1. The proposed sensor was successfully applied in the determination of levofloxacin in urine, and the obtained results were in full agreement with those from the HPLC procedure.     

Determination of levofloxacin and norfloxacin by capillary electrophoresis with electrochemiluminescence detection and applications in human urine

A novel method for the determination of norfloxacin (NOR) and levofloxacin (LVX) was developed by CE separation and electrochemiluminesence detection (ECL). The methods for capillary conditioning and the effect of solvent type were studied. Parameters affecting the CE and ECL were also investigated. Under the optimum conditions, the two analytes were well separated within 9 min. The LODs (S/N = 3) in standard solution are 4.8 x 10(-7) mol/L for NOR and 6.4 x 10(-7) mol/L for LVX, respectively. The precisions of intraday and interday are less than 4.2 and 8.1%, respectively. The LOQs (S/N = 10) in real human urine samples are 1.2 x 10(-6) mol/L for NOR and 1.4 x 10(-6) mol/L for LVX, respectively. The applicability of the proposed method was illustrated in the determination of NOR and LVX in human urine samples and the monitoring of pharmacokinetics for NOR. The recoveries of NOR and LVX at different levels in human urine samples were between 84.3 and 92.3%.