毛细管电泳法分析食品和体液中氟喹诺酮类药物残留
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摘要
喹诺酮是一类重要的广谱抗菌药,已经广泛应用于医学和兽医学中。该类药物在被大量使用的同时带来了与健康安全相关的问题,因此对喹诺酮的分析研究已经引起人们的重视。建立操作简便,灵敏,可靠的喹诺酮类药物分析以及在食品和体液中残留分析的方法日趋迫切。毛细管电泳技术具有高效,微量,污染小以及分析速度快等优点,在药物分析中的应用日益广泛,在喹诺酮类药物分析中也发挥了越来越重要的作用。
第一章：概括了兽药残留分析的重要性,对喹诺酮类药物的概况进行了简述,并就喹诺酮类药物的毛细管电泳法分析现状进行了综合评述。
第二章：建立了一种快速分离和同时测定复方乳酸环丙沙星注射液中环丙沙星和利巴韦林配伍药的毛细管区带电泳新方法。考察了缓冲溶液pH值,浓度,电压,温度等电泳条件,线性良好,两种物质得到有效分离。实验结果表明,所建方法能够用于药物制剂中环丙沙星和利巴韦林的同时定量测定。
第三章：对快速分离和同时测定人体尿液中加替沙星、洛美沙星、依诺沙星、环丙沙星、氧氟沙星、恩诺沙星、氟罗沙星和培氟沙星这8种氟喹诺酮的毛细管区带电泳新方法进行了研究,用二极管阵列检测器检测。分别考察了缓冲溶液pH值,浓度,电压,温度等因素对8种氟喹诺酮药物分离的影响。在最佳实验条件下线性良好,8种药物可以得到基线分离。可用于尿液中8种氟喹诺酮的常规检测。
第四章：用毛细管电泳法结合固相萃取前处理技术分离并测定了牛奶和蜂蜜中的沙拉沙星,恩诺沙星,环丙沙星和氟罗沙星。本实验对缓冲溶液,温度,电压进行了考查和优化。用0.1 mol／L-1EDTA／McIlvaine buffer(pH 4.0)沉淀牛奶,提取氟喹诺酮药物,而用盐酸水溶液(pH3)溶解蜂蜜。样品经Oasis HLB柱净化,不存在杂质干扰。本方法净化系统简单,分析时间短,能够用于牛奶和蜂蜜中氟喹诺酮的定量测定。
The quinolones are considered the most important group of synthetic antibacterial drugs, and they are widely used in human and veterinary medicine. The wide usage of antibiotics may be responsible for the promotion of resistant stains of bacteria, but the misuse of these pharmaceuticals and the residues may given rise to public health, the analysis of quinolones attracts people's attentions. So it is urgent to development methods for the determination of quinolones and its residues in food and fluid. Capillary electrophoresis (CE) has become a very important technique for pharmaceutical analysis because of its high separation efficiency, little of environmental pollution, high speed and small sample volume requirements.
Chapter one:The significance of veterinary residue analysis is summarized, Bases of quinolones are introduced briefly, and the applications of capillary electrophoresis methods for the determination of quinolones are reviewed.
Chapter two:A method has been established for the simultaneous determination of ciprofloxacin (CIP) and Ribavirin. The effects of pH, concentration of buffer, temperature and voltage on the separation of the analytes were investigated. The calibration curve has good linearity and the two drugs are baseline separated easily. This method has been successfully applied to simultaneous determination of CIP and Ribavirin in the pharmaceutical preparations. The proposed method can be applied for routine quantification of studied drugs.
Chapter three:The work in order to develope a simple, rapid and accurate method for effective separation and simultaneous determination of gatifloxacin, lomefloxacin, enoxacin, ciprofloxacin, ofloxacin, enrofloxacin, flumequine and pefloxacin residues in urine by capillary electrophoresis with diode-array detector. Study on the effects of pH, concentration of buffer, voltage and temperature to the separation of the fluoroquinolones. It has good linearity and the fluoroquinolones are baseline separated in the best electrophoresis conditions. This method has been successfully applied for routine determination of the eight fluoroquinolones in urine samples.
Chapter four:A capillary electrophoresis method with solid phase extraction are developed for the determination of Sarafloxacin, ciprofloxacin, enrofloxacin and flumequine in milk and honey. Separation conditions of capillary electrophoresis, including running buffer, voltage and temperature, are investigated and optimized. This work has shown that 0.1 mol L-1EDTA in McIlvaine buffer at pH 4.0 is efficient agent for extracting the analytes in milk, the water adjusted with 0.1M HCL(pH 3)as solvent to dissolve the honey. This method in which SPE treatment with Oasis HLB cartridges is used as a clean-up step for obtaining a background free of interferences in the electropherograms of real samples, successfully separated and determined the four fluoroquinolones in milk and honey samples. The proposed method has short analysis time, simple clean-up system, high detection capability, and can be applied to monitor structurally related novel fluoroquinolone antibiotics in milk and honey.
第一章：概括了兽药残留分析的重要性,对喹诺酮类药物的概况进行了简述,并就喹诺酮类药物的毛细管电泳法分析现状进行了综合评述。
第二章：建立了一种快速分离和同时测定复方乳酸环丙沙星注射液中环丙沙星和利巴韦林配伍药的毛细管区带电泳新方法。考察了缓冲溶液pH值,浓度,电压,温度等电泳条件,线性良好,两种物质得到有效分离。实验结果表明,所建方法能够用于药物制剂中环丙沙星和利巴韦林的同时定量测定。
第三章：对快速分离和同时测定人体尿液中加替沙星、洛美沙星、依诺沙星、环丙沙星、氧氟沙星、恩诺沙星、氟罗沙星和培氟沙星这8种氟喹诺酮的毛细管区带电泳新方法进行了研究,用二极管阵列检测器检测。分别考察了缓冲溶液pH值,浓度,电压,温度等因素对8种氟喹诺酮药物分离的影响。在最佳实验条件下线性良好,8种药物可以得到基线分离。可用于尿液中8种氟喹诺酮的常规检测。
第四章：用毛细管电泳法结合固相萃取前处理技术分离并测定了牛奶和蜂蜜中的沙拉沙星,恩诺沙星,环丙沙星和氟罗沙星。本实验对缓冲溶液,温度,电压进行了考查和优化。用0.1 mol／L-1EDTA／McIlvaine buffer(pH 4.0)沉淀牛奶,提取氟喹诺酮药物,而用盐酸水溶液(pH3)溶解蜂蜜。样品经Oasis HLB柱净化,不存在杂质干扰。本方法净化系统简单,分析时间短,能够用于牛奶和蜂蜜中氟喹诺酮的定量测定。
The quinolones are considered the most important group of synthetic antibacterial drugs, and they are widely used in human and veterinary medicine. The wide usage of antibiotics may be responsible for the promotion of resistant stains of bacteria, but the misuse of these pharmaceuticals and the residues may given rise to public health, the analysis of quinolones attracts people's attentions. So it is urgent to development methods for the determination of quinolones and its residues in food and fluid. Capillary electrophoresis (CE) has become a very important technique for pharmaceutical analysis because of its high separation efficiency, little of environmental pollution, high speed and small sample volume requirements.
Chapter one:The significance of veterinary residue analysis is summarized, Bases of quinolones are introduced briefly, and the applications of capillary electrophoresis methods for the determination of quinolones are reviewed.
Chapter two:A method has been established for the simultaneous determination of ciprofloxacin (CIP) and Ribavirin. The effects of pH, concentration of buffer, temperature and voltage on the separation of the analytes were investigated. The calibration curve has good linearity and the two drugs are baseline separated easily. This method has been successfully applied to simultaneous determination of CIP and Ribavirin in the pharmaceutical preparations. The proposed method can be applied for routine quantification of studied drugs.
Chapter three:The work in order to develope a simple, rapid and accurate method for effective separation and simultaneous determination of gatifloxacin, lomefloxacin, enoxacin, ciprofloxacin, ofloxacin, enrofloxacin, flumequine and pefloxacin residues in urine by capillary electrophoresis with diode-array detector. Study on the effects of pH, concentration of buffer, voltage and temperature to the separation of the fluoroquinolones. It has good linearity and the fluoroquinolones are baseline separated in the best electrophoresis conditions. This method has been successfully applied for routine determination of the eight fluoroquinolones in urine samples.
Chapter four:A capillary electrophoresis method with solid phase extraction are developed for the determination of Sarafloxacin, ciprofloxacin, enrofloxacin and flumequine in milk and honey. Separation conditions of capillary electrophoresis, including running buffer, voltage and temperature, are investigated and optimized. This work has shown that 0.1 mol L-1EDTA in McIlvaine buffer at pH 4.0 is efficient agent for extracting the analytes in milk, the water adjusted with 0.1M HCL(pH 3)as solvent to dissolve the honey. This method in which SPE treatment with Oasis HLB cartridges is used as a clean-up step for obtaining a background free of interferences in the electropherograms of real samples, successfully separated and determined the four fluoroquinolones in milk and honey samples. The proposed method has short analysis time, simple clean-up system, high detection capability, and can be applied to monitor structurally related novel fluoroquinolone antibiotics in milk and honey.
引文
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