Synchronous fluorescence determination of ciprofloxacin in the pharmaceutical formulation and human serum based on the perturbed luminescence of rare-earth ions

A simple, rapid and sensitive synchronous fluorescence method was developed for the determination of ciprofloxacin (CPFX) in the pharmaceutical formulation and human serum. The results show that when Y³⁺ is added into the CPFX solution, the characteristic fluorescence of Y³⁺ is not emitted whereas the fluorescence intensity of CPFX is significantly enhanced. The synchronous fluorescence technology is employed in this method to directly determine trace amount of CPFX in human serum. A linear relationship between the fluorescence intensity and the CPFX concentration is obtained in the range of 1.0×10⁻⁹ ∼5.0×10⁻⁶ mol L⁻¹. The limit of detection (LOD) of this method attains as low as 2.0×10⁻¹⁰ mol L⁻¹ (S/N=3). The selectivity of this method is also very good. Common metal ions, rare-earth ions and some pharmaceuticals, which are usually used together with CPFX in the clinic, do not interfere with the determination of CPFX under general conditions.     

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.     

氨酚伪麻那敏片3成分含量测定法

建立氨酚伪麻那敏片中的对乙酰氨基酚、盐酸伪麻黄碱和马来酸氯苯那敏含量测定的方法.采用C18柱（4.6mm×250mm,5μm）,以磷酸三乙胺溶液（pH 2.5）为流动相,流速为1mL·min-1,检测波长为215nm,进样量为20μL.盐酸伪麻黄碱在201.7-4034.0ng、对乙酰氨基酚在101.5-2031.0ng,马来酸氯苯那敏20.8-415.5ng与峰面积线性关系良好,平均回收率（n=9）分别为100.0％（RSD为2.0％）、101.0％ （RSD为0.5％）、99.5％（RSD为0.7％）.该法一个液相色谱系统可同时测定上述3种成分,简便、准确、专属,可用于氨酚伪麻那敏片的含量测定.     

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.     

Gran电位滴定法测定乳酸环丙沙星

介绍了乳酸环丙沙星测定的Gran电位滴定法。采用Gran线性函数进行电位滴定,经图解外推或线性回归处理求出计量点,可直接用于测定乳酸环丙沙星原料药的含量。该法用于多批原料药的测定,结果与药典法基本一致。     

高效液相色谱法测定盐酸倍他司汀片的有关物质

采用Kromasil C18分析柱,水-乙腈(体积比为68：32)混合液为流动相,流速为1．0ml/min,检测波长为261nm,用高效液相色谱法测定盐酸倍他司汀片的有关物质。盐酸倍他司汀样品溶液中有关物质的色谱峰面积之和及2％盐酸倍他司汀线性对照溶液中主成分的色谱峰面积均与盐酸倍他司汀的浓度线性相关,相关系数分别为0．9991、0.9997。     

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。     

盐酸环丙沙星分子印迹电化学传感器

本文将电化学合成与分子印迹技术相结合,采用循环伏安法在石墨电极表面,形成盐酸环丙沙星(CPX)分子印迹聚吡咯薄膜,制备了CPX分子印迹传感器。实验对传感器的制备条件进行了优化,用铁氰化钾作为活性电子探针,采用方波伏安法研究了传感器性能。结果表明,在1×10~(-8)~1×10~(-4)mol/L范围内,峰电流与CPX浓度负对数呈良好的线性关系,检出限(S/N=3)为3.5×10~(-9)mol/L。传感器对模板分子CPX选择性强,重现性和稳定性好,置于室温下15d峰电流强度无明显变化。     

Formation of Oxygen Vacancies on the {010} Facets of BiOCl and Visible Light Activity for Degradation of Ciprofloxacin

BiOCl nanosheets with oxygen vacancies on the exposed {010} facets were assistant-synthesized by triethanolamine(TEOA) via hydrothermal method. We explored the surface properties, crystal structure, morphology and optical absorption ability of the prepared samples via various characterization technologies. The results indicate that the morphologies and microstructures of the obtained samples depend on the amount of TEOA in the synthesis. The addition of TEOA induces the production of oxygen vacancy on the surface of the samples. Therefore, the synthesized samples with TEOA-assistance hold higher photoactivity for the degradation of colorless antibiotic agent ciprofloxacin(CIP) under visible light(λ ≥ 420 nm). The obtained sample upon the addition of 20 mL of TEOA exhibits the highest photocatalytic performance, which is nearly 14 times as high as that of the sample prepared without TEOA and twice as high as that of the prepared samples with NaOH or NH₃·H₂O. The possible degradation mechanism was discussed on the basis of the experiment results.     

流动注射抑制化学发光法测定盐酸环丙沙星

在碱性介质中,环丙沙星对鲁米诺-KIO4-Co2 反应体系产生的化学发光明显地受到抑制,且化学发光强度的抑制强度与环丙沙星的浓度成正比关系.基于上述现象,提出了环丙沙星的流动注射-化学发光测定法.环丙沙星的质量浓度在3.0×10-7～1.0×10-5g·L-1之间成线性关系,检出限为2.0×10-7g·L-1.对浓度水平为1.0×10-6g·L-1的盐酸环丙沙星进行11次平行测定,得到RSD(n=11)值为2.7%.应用此方法分析了环丙沙星药片,所得结果与按中国药典方法所得测定值保持一致,回收率试验的结果在98.5%～101.2%之间.