甲磺酸培氟沙星荷移反应及荧光光谱性质研究

研究了甲磺酸培氟沙星与电子受体四氯对苯醌之间的荷移反应 ,实验表明 ,在甲醇体系中 ,甲磺酸培氟沙星与四氯对苯醌在光的作用下可形成稳定的荷移络合物 ,其荧光发射强度较甲磺酸培氟沙星显著增强 ,且最大激发波长和发射波长向长波方向分别位移 80和 6 0nm。在 0 0 5～ 10 μmol·L-1浓度范围内 ,甲磺酸培氟沙星荧光强度与浓度呈良好线性关系 ,其检出限为 0 0 0 4 μmol·L-1。该方法用于甲磺酸培氟沙星胶囊中甲磺酸培氟沙星含量的测定 ,结果与紫外 可见光度法一致。     

培氟沙星-铽(Ⅲ)-牛血清白蛋白体系的荧光光谱及其应用

在pH 8.2的Tris-HCl缓冲溶液中, Tb3+与培氟沙星(PEFX)形成的配合物受290 nm紫外光激发发出Tb3+的特征荧光峰, 加入牛血清白蛋白(BSA)能大大增强体系的荧光强度, 由此建立了PEFX-Tb3+ 配合物探针测定BSA的方法. 与PEFX-Tb3+二元配合物相比, PEFX-Tb3+-BSA三元体系荧光强度显著增强. 研究了反应的最佳条件, 并对PEFX-Tb3+-BSA荧光增强作用的机理进行了探讨.     

甲磺酸培氟沙星在胶束中的荧光特性研究及应用

在弱酸性介质中,十二烷基硫酸钠(SDS)对甲磺酸培氟沙星有较强的增敏作用,据此建立了胶束增敏荧光光谱法测定痕量甲磺酸培氟沙星的分析方法。本法的线性范围为0.01~1.63mg.L-1,检出限为6.0×10-3μg.mL-1,回收率为99.8%~101.7%,相对标准偏差为0.43%~1.34%。     

Investigation on enhanced chemiluminescence reaction systems with bis(hydrogenperiodato) argentate(III) complex anion for fluoroquinolones synthetic antibiotics

A novel chemiluminescence (CL) reaction system with bis(hydrogenperiodato) argentate(III) complex anion (Ag(III) complex, [Ag(HIO₆)₂]⁵⁻), for the first time, is developed for the determination of lomefloxacin (LMFX), enrofloxacin (ENLX) and pefloxacin (PFLX). The possible CL emission mechanism was discussed by comparing the fluorescence emission with CL spectra. The CL conditions of [Ag(HIO₆)₂]⁵⁻-H₂SO₄-LMFX/ENLX/PFLX systems were investigated and optimized. Under the optimized experimental conditions, the CL intensity is proportional to the concentration of the drugs in the range 0.2994-36.80 × 10⁻⁷ g mL⁻¹ for LMFX, 4.00-30.0 × 10⁻⁷ g mL⁻¹ for ENLX and 1.54-27.64 × 10⁻⁷ g mL⁻¹ for PFLX. The limit of detection (s/n = 3) was 9.1 × 10⁻⁹ g mL⁻¹ for LMFX, 3.1 × 10⁻⁹ g mL⁻¹ for ENLX and 4.4 × 10⁻⁹ g mL⁻¹ for PFLX. The recovery of LMFX, ENLX and PELX from the spiked pharmaceutical preparations was in the range of 92.3-105% with the RSDs of 0.5-2.7%. For urine, serum and milk samples the recoveries of the three drugs were in the range of 85.1-107% for LMFX with the RSDs of 2.3-3.4%. 80.2-112% for ENLX with the RSDs of 1.4-2.8%, and 87.8-114% for PFLX with the RSDs of 1.6-2.7%. The proposed method was applied successfully to the determination of these compounds in real samples.     

培氟沙星胶束包合物的荧光特性及应用

提出一种基于胶束增敏测定培氟沙星的荧光分光光度法 ,研究了培氟沙星与十二烷基硫酸钠 (SDS)形成胶束包合物的荧光性质 ,对影响荧光的不同变量和参数进行了研究和优选。试验结果表明 ,在pH 5的BrittonRobinson(BR)缓冲溶液中 ,SDS胶束对培氟沙星有强的增敏作用 ,培氟沙星胶束包合物的激发和发射波长分别为 λex =2 78nm和λem =4 32nm 。其线性范围为 0 0 6～ 1 2 0 μg·mL- 1 ,方法检出限为 0 0 6 μg·mL- 1 ,回收率为 98 5 %～ 10 0 8% ,相对标准偏差为 1 4 %～ 2 3%。该方法已成功用于片剂和血浆中培氟沙星含量的测定 ,其结果令人满意。本文采用同步导数荧光光谱法测定了血浆中的培氟沙星 ,其选择性好 ,灵敏度高 ,可有效地消除血浆中荧光背景的干扰 ,降低了检测限。     

基于THz-TDS技术的培氟沙星和氟罗沙星抗生素定性定量检测研究

作为两种常用的喹诺酮类抗生素,培氟沙星和氟罗沙星残留问题引起人们的高度关注,研发快速、高效的检测手段成为一种需求。采用太赫兹时域光谱(THz-TDS)技术对鱼粉基质中的培氟沙星、氟罗沙星进行了研究。制备培氟沙星、氟罗沙星、聚乙烯和鱼粉纯净物质以及培氟沙星-鱼粉和氟罗沙星-鱼粉17种不同浓度二元混合物的压片样品,共106个;对所有压片样品进行太赫兹光谱测量和分析;利用连续投影算法(SPA)结合支持向量机(SVM)和反向传播神经网络(BPNN)建立定性判别模型,对培氟沙星-鱼粉和氟罗沙星-鱼粉这两种混合物进行分类判别;利用特征频率处吸收系数建立偏最小二乘回归(PLSR)、BPNN、多元线性回归(MLR)定量预测模型,分别对两种混合物进行定量预测。结果表明：纯净培氟沙星在0.775和0.988 THz存在明显吸收峰,纯净氟罗沙星在0.919和1.088 THz存在明显吸收峰,聚乙烯对太赫兹波基本没有吸收,鱼粉无吸收峰,两种抗生素与鱼粉混合后的峰值出现在纯净抗生素的吸收峰附近;在定性判别中,SVM判别结果最佳,预测集判别准确率、精确率、召回率、F1得分分别为97.06%,97.22%,97.06%和97.06%;定量回归中,SPA-BPNN 模型用于预测培氟沙星-鱼粉结果最佳,预测集相关系数(R_p)、预测集均方根误差(RMSEP)分别为0.984 9和0.009 5,SPA-MLR模型用于预测氟罗沙星-鱼粉结果最佳,R_p和RMSEP分别为0.982 7和0.040 6。研究表明THz-TDS技术对鱼粉基质中培氟沙星、氟罗沙星进行定性定量检测是可行的,为畜禽行业中培氟沙星和氟罗沙星实际检测提供理论和技术参考。     

甲磺酸培氟沙星的极谱研究与测定

甲磺酸培氟沙星在０．１０ｍｏｌ／Ｌ的Ｎａ２ＨＰＯ４－ＫＨ２ＰＯ４缓冲液中，于－１．４９Ｖ处产生一灵敏的二了介导数还原波，极谱波的峰电位不受溶液ＰＨ值的影响，该峰对应于芳香酮的还原。     

Multicomponent kinetic spectrophotometric determination of pefloxacin and norfloxacin in pharmaceutical preparations and human plasma samples with the aid of chemometrics

A spectrophotometric method for the simultaneous determination of the important pharmaceuticals, pefloxacin and its structurally similar metabolite, norfloxacin, is described for the first time. The analysis is based on the monitoring of a kinetic spectrophotometric reaction of the two analytes with potassium permanganate as the oxidant. The measurement of the reaction process followed the absorbance decrease of potassium permanganate at 526nm, and the accompanying increase of the product, potassium manganate, at 608nm. It was essential to use multivariate calibrations to overcome severe spectral overlaps and similarities in reaction kinetics. Calibration curves for the individual analytes showed linear relationships over the concentration ranges of 1.0-11.5mgL(-1) at 526 and 608nm for pefloxacin, and 0.15-1.8mgL(-1) at 526 and 608nm for norfloxacin. Various multivariate calibration models were applied, at the two analytical wavelengths, for the simultaneous prediction of the two analytes including classical least squares (CLS), principal component regression (PCR), partial least squares (PLS), radial basis function-artificial neural network (RBF-ANN) and principal component-radial basis function-artificial neural network (PC-RBF-ANN). PLS and PC-RBF-ANN calibrations with the data collected at 526nm, were the preferred methods-%RPE(T) approximately 5, and LODs for pefloxacin and norfloxacin of 0.36 and 0.06mgL(-1), respectively. Then, the proposed method was applied successfully for the simultaneous determination of pefloxacin and norfloxacin present in pharmaceutical and human plasma samples. The results compared well with those from the alternative analysis by HPLC.     

培氟沙星-Al(Ⅲ)配合物与DNA的相互作用研究

利用荧光和紫外光谱法研究了培氟沙星(PEF)-Al3 配合物与DNA的相互作用.培氟沙星(PEF)能与Al3 生成PEF-Al(Ⅲ)二元配合物,该配合物能与DNA发生相互作用.利用DNA与PEF-Al(Ⅲ)作用能猝灭体系荧光强度的性质测定DNA,其线性范围为8.0×10-6～2.25×10-4 mol/L,检出限为5.0×10-6 mol/L.讨论了反应的最佳条件及其结合机理.     

Spectroscopic and voltammetric studies of Pefloxacin bound to calf thymus double-stranded DNA

Spectral and electrochemical studies have been carried out on the interaction of pefloxacin with calf thymus double-stranded dsDNA. The voltammetric behavior of pefloxacin was investigated at glassy carbon, carbon paste and dsDNA-modified carbon paste electrodes using cyclic voltammetry. Pefloxacin was oxidized, yielding one irreversible oxidation peak. The modification of the carbon paste surface with dsDNA allowed an accumulation process to take place for pefloxacin such that higher sensitivity was achieved compared with the bare surface. The response was characterized with respect to ionic strength, accumulation time, pefloxacin concentration, and other variables. The stripping differential pulse voltammetric response showed a linear calibration curve in the range 1.0×10^–7–1.0×10^–5 mol l^–1 with a detection limit of 5.0×10^–8 mol l^–1 at the dsDNA modified electrode. The method was applied to the direct determination of pefloxacin in diluted urine samples.