铽-环丙沙星与罗丹明B间稀土敏化荧光能量转移机理研究

利用荧光光谱法及紫外光谱法研究发现pH6.2醋酸-醋酸钠(HAc-NaAc)水溶液中铽与环丙沙星形成络合物使铽在490,545,590nm处出现Tb3 的特征发射峰即荧光被强烈的敏化增强,且在545nm处的荧光强度最大,铽离子的锐线发射光谱的特征最强峰545nm与罗丹明B的最大吸收峰波长552nm十分接近,能够发生能量转移反应。因此,随着碱性染料罗丹明B的加入铽-环丙沙星的特征荧光呈现有规律降低,表明罗丹明B对铽-环丙沙星荧光有猝灭作用,研究结果表明其猝灭类型主要为静态猝灭。又根据Frster理论,测得了罗丹明B对铽-环丙沙星的能量转移效率,相互结合距离等参数。从而进一步证明了该反应是单一静态猝灭过程,阐述了其荧光猝灭机理是通过能量转移产生的。     

高效液相色谱法检测冷冻烤鳗中恩诺沙星等药物残留

论述了高效液相色谱法检测冷冻烤鳗中恩诺沙星、环丙沙星、诺氟沙星等合成抗菌剂残留的方法。样品以乙腈为提取剂,经脱脂、浓缩、净化,用流动相溶解。高效液相色谱荧光检测器测定。各标准曲线线性范围为0.005～1.000mg·kg-1,回收率为86.2%～92.3%,检出限分别为1,2,2μg·kg-1。     

Simple and cost-effective determination of ciprofloxacin hydrochloride by electrical micro-titration

By employing an electrical micro-titration system, in which a capacitively coupled contactless conductivity detector(C4D) was used to monitor the reaction process in real time, herein a novel method for determining ciprofloxacin hydrochloride(CIPHCl) was developed for the first time. Mode 1: Standard CIPHCl solutions at different concentrations were loaded into reaction cells, respectively, and were titrated with standard Ag+. Upon the titration, the formation of a precipitate alters the number of ions in the solution, raising the change of conductivity, which was monitored by a special C~4 D to construct a titration curve. The endpoint of the titration was located from the peak of the curve. Between the elapsed time and the initial concentration of titrand, a linear relationship was established over the range of2.0–8.0 mmol/L. Mode 2: Standard Fe~(3+) took the place of Ag~+, and was used as titrant to recognize ciprofloxacin contributed to the formation of complexation, which also resulting a change of solution conductivity. Under optimized conditions, a working range of 1.0–5.0 mmol/L CIPHCl was found. Because the reaction solutions were isolated from the working electrodes, this pioneer work shows significant simplicity and cost-effectiveness, by eliminating the requirements for detector exchange/renewal between different measurements, and by involving no auxiliary chemicals. Both of the two approaches were applied successfully to determine CIPHCl in tablet samples. And the results were in good agreement with those obtained by reference method.     

High-throughput measurements of ciprofloxacin,clomipramine and fexofenadine hydrochlorides with an 8-channel electrical titrator

By employing a developed automatic eight-channel electrical titrator, ciprofloxacin, clomipramine and fexofenadine hydrochlorides are determined in batch, respectively, with satisfactory accuracy and precision. It shows a higher efficiency superior to traditional titration method, and maximally 30 measurements per minute can be completed.     

Determination of enrofloxacin and its metabolite ciprofloxacin by high performance capillary electrophoresis with end-column amperometric detection

Enrofloxacin (ENR) and its metabolite ciprofloxacin (CIP) were determined by capillary zone electrophoresis (CZE) with end-column amperometric detection. The effect of several factors, such as pH and concentration of running buffer solution, separation voltage, injection time, and working potential, on CZE were investigated to establish the optimal conditions of separation and detection. Under a given set of conditions (pH 8.00 phosphate buffer solution (20 mmol/L); +0.95 V for the working potential; 18 kV for the separation voltage; sample injection at 18 kV for 10 s), the compounds investigated can be well separated and detected within 8 min. Excellent linearity was observed between peak currents and concentration of analytes in the range from 0.034 to 70.0 mg/kg for these two compounds. The detection limits (S/N= 3) for enrofloxacin and ciprofloxacin were 13.68 mg/kg and 14.35 mg/kg, respectively, which were about 7-fold lower than the maximum residue limits (MRLs) established by the European Union. A simple sample pretreatment method was developed and proved to be effective in obtaining good recoveries and short analysis time. The developed CE-AD method was simpler, faster, and less cost intensive than other reported methods, and allows the determination of ENR and its metabolite CIP in contaminated eel liver samples and other animal tissue samples at the required maximum residue limits.     

A liquid chromatographic method, with fluorometric detection, for the determination of enrofloxacin and ciprofloxacin in plasma and endometrial tissue of mares

The aim of this work was to develop and validate a simple and sensitive analytical method for determining enrofloxacin (EFX) and ciprofloxacin (CFX) in equine plasma and endometrial tissue samples, as a precursor to conducting pharmacokinetic/pharmacodynamic studies on equine endometritis This was achieved in the form of a liquid chromatographic procedure, with fluorometric detection, which also gave good separation of other fluoroquinolones including marbofloxacin (MFX), danofloxacin (DFX) and ofloxacin (OFX). Analytes were separated on a C₁₈ reversed phase column using an acidified mobile phase. The exact composition of the mobile phase differed for plasma (16% acetonitrile:methanol [13:1,v/v] 84% water containing 0.4% triethylamine and 0.4% phosphoric acid [35%]) and endometrial tissue (14% acetonitrile, 86% water, without methanol) samples. EFX and CFX were both detected at excitation and emission wavelengths of 294 and 500 nm, respectively. Prior to chromatography, EFX and CFX were purified by solid phase extraction from plasma, and a combination of solvent/solid phase extraction from endometrial tissue.

Mean absolute recoveries for EFX and CFX from plasma were 94.1 and 78.0%, respectively, and from endometrial tissue, 78.0 and 57.8%, respectively, with a percentage residual standard deviation (%R.S.D.) <10% in each case. Mean relative recoveries for EFX and CFX from plasma were 91.3 and 119.4%, respectively, and from endometrial tissue, 80.2 and 108.0%, respectively, with a %R.S.D. <20% in each case.

Standard curves constructed using blank plasma and endometrial tissue samples, spiked with authentic EFX and CFX in the ranges 0.005–10.0 μg mL⁻¹ and 0.05–10.0 μg g⁻¹, respectively, all showed acceptable linearity with correlation coefficients, r² ≥ 0.977. Mean intra- and inter-day precision (expressed as %R.S.D.) was <6 and <13%, respectively, with an associated accuracy (expressed as percentage relative error, %R.E.) of <20% for both analytes in both matrices. Acceptable precision and accuracy was also demonstrated at the pre-assigned LOQs of 0.005 μg mL⁻¹ for both EFX and CFX in plasma, and 0.05 μg g⁻¹ for both drugs in endometrial tissue. EFX and CFX were stable in both plasma and endometrial tissue for at least 60 days at −20 °C.     

Determination of Ciprofloxacin,Enrofloxacin, and Marbofloxacin in Bovine Urine,Serum, and Milk by Microextraction by a Packed Sorbent Coupled to Ultra-High Performance Liquid Chromatography

This article reports new, easy, and rapid microextraction by packed sorbent (MEPS)–ultra high performance liquid chromatography with photodiode array detection for the simultaneous determination in bovine urine, serum, and milk of three antibiotics belonging to the class of the fluoroquinolones, namely ciprofloxacin, enrofloxacin, and marbofloxacin, approved for veterinary and human use (ciprofloxacin). The chromatographic separation of the analytes and all aspects influencing the MEPS performance were optimized for the extraction from the considered biological samples. The optimized procedure required simple sample pretreatment, a short (<8?min) isocratic elution, and provided sufficient sensitivity for the determination of the analytes at trace levels in compliance with current legislation. Limits of quantitation were in the range from 0.002 (ciprofloxacin, urine) to 0.048?μg/mL (enrofloxacin, milk). Recoveries from 79% (enrofloxacin, milk) to 88% (ciprofloxacin, urine/serum) were obtained on spiked samples. The within-day (n?=?6) and between-day (n?=?6 over 3?days) relative standard deviation percentages in bovine urine, serum, and milk samples ranged from 2.2 (ciprofloxacin, urine) to 2.5 (enrofloxacin, serum) and from 3.1 (ciprofloxacin, urine) to 3.7 (enrofloxacin, milk), respectively, and were not concentration dependent. To the best of our knowledge, this is the first study describing a fast and simple method for the determination of fluoroquinolones in bovine biological samples.     

盐酸环丙沙星的示波极谱测定及其机理研究

在ＰＨ６．９的ＫＨ２ＰＯ４－ＫＯＨ缓冲液中，盐酸环丙沙星在滴汞电极上产生一灵敏的催化氢波。峰电位为－１．５１Ｖ，在１．００×１０＾－７－２．００×１０＾－５ｍｏｌ．Ｌ＾－１之间有良好的线性关系，用于对盐酸环丙沙星的测定，方法简便、结果准确可靠。     

Efficient loading and delivery of ciprofloxacin by smart alginate/carboxylated graphene oxide/aminated chitosan composite microbeads: In vitro release and kinetic studies

New composite microbeads were formulated as smart pH-sensitive vehicle for efficient delivery of ciprofloxacin (CIP) drug. Herein, carboxylated graphene oxide (CGO) was successfully impregnated into alginate (Alg) microbeads, which were then coated with aminated chitosan (AmCs) layer to form core–shell Alg/CGO@AmCs composite microbeads. Diverse analysis tools comprising FTIR, TGA, XRD and SEM were employed to characterize the developed carriers, while their swelling profiles and pH-sensitivity were examined under different pHs. The results clarified that increasing CGO and AmCs concentrations in microbeads matrix greatly protected Alg microbeads from fast disintegration at colon pH and prolonged their swelling time. Moreover, about 94.65 % of CIP drug was successfully loaded by Alg/CGO@AmCs composite microbeads compared to 61.95 % for Alg microbeads, confirming their reduced porosity. The in vitro CIP-release profiles were investigated in simulated gastrointestinal conditions. Furthermore, increasing AmCs concentration in the outer shell of composite microbeads clearly minimized the CIP burst release at the colon region and offered a sustained release performance. Besides, the CIP release mechanism was well-described by korsmeyer-peppas kinetic model. The cytotoxicity study confirmed the potential safety of the Alg/CGO@AmCs composite microbeads with human cell viability reached 98.98 %, suggesting their applicability as smart carriers for oral delivery of antibiotics.     

盐酸环丙沙星三元配合物体系的光谱研究及应用

研究了盐酸环丙沙星、茜素和稀土镧离子所形成的三元配合物体系。结果表明,以水-乙醇作为溶剂,在pH为5.8的KH2PO4-NaOH缓冲液中,该三元配合物最大吸收波长为280 nm,表观摩尔吸收系数为4.23×104L.mol-1.cm-1,盐酸环丙沙星在0.3~34.5 mg/L范围内符合郎伯-比耳定律,方法的检出限为0.01 mg/L。已用于市售盐酸环丙沙星片和胶囊的测定。