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氟甲喹单克隆抗体制备、鉴定及间接竞争酶联免疫吸附分析法 总被引:1,自引:0,他引:1
以氟甲喹(FLU)为原料,合成4个碳原子手臂的半抗原(FLUABA),采用活泼酯法与牛血清白蛋白(BSA)偶联制备免疫抗原,通过免疫Balb/c小鼠及细胞融合,获得1株稳定分泌抗氟甲喹单克隆抗体的杂交瘤细胞株DB6-E7,其抗体亚类为IgG1,亲和力常数(KA)为8.19×108L/mol。将氟甲喹、FLUABA及6个碳原子手臂的半抗原FLUACA分别与卵清白蛋白(OVA)偶联作为包被抗原,研究异源包被对间接竞争ELISA灵敏度的影响。结果表明,异源包被可显著提高ELISA方法的灵敏度。基于最佳异源包被(FLU-OVA)的酶联免疫吸附分析法的IC50为26.33μg/L,检出限为4μg/L,定量检测范围为8.0~114μg/L(IC20~IC80)。与喹诺酮类药物及结构类似物几乎不存在交叉反应,特异性高。此方法可满足畜禽产品中氟甲喹残留的快速筛查。 相似文献
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A highly enantioselective organocatalytic transfer hydrogenation enabling the synthesis of both 6-fluoro-2-methyltetrahydroquinoline and 7,8-difluoro-3-methyl-benzoxazine has been developed. These key building blocks can for the first time be synthesized using the same methodology allowing fast and efficient, metal-free access to the antibiotic fluoroquinolones flumequine and levofloxacine. 相似文献
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Determination and on-line clean-up of (fluoro)quinolones in bovine milk using column-switching liquid chromatography fluorescence detection 总被引:1,自引:0,他引:1
A simple, cost-effective, and high throughput method using on-line column-switching liquid chromatography fluorescence detection was developed and validated for analysing five (fluoro)quinolones (FQs)--enrofloxacin (ENRO), ciprofloxacin (CIPR), sarafloxacin (SARA), oxolinic acid (OXOL), and flumequine (FLUM) in bovine milk. Norfloxacin (NORF) and nalixidic acid (NALI) were used as internal standards. After simple deproteination of milk sample with 5% (w/v) metaphosphoric acid, the supernatant was subject to on-line column clean-up and direct analysis by LC-FLD. The extraction cartridge was prepared in-house by slurry packing with hydrophilic-lipophilic polymer sorbent. The accuracy of measurement for each (fluoro)quinolone at different maximum residue limits (MRL) was 101-103% (ENRO), 92.8-97.4% (CIPR), 89.8-92.8% (SARA), 116-121% (OXOL), and 81.3-85.5% (FLUM), whilst the precision was 2.9-6.1% (ENRO), 2.5-5.1% (CIPR), 2.3-5.0% (SARA), 3.1-5.9% (OXOL), and 5.6-6.5% (FLUM). The decision limits, detection capabilities, specificity and analytes stability during storage were also investigated. 相似文献
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In this work the viability of a fluorescent technique for the determination of quinolones is studied. This analytical technique allows one to analyze the effect of the increasing order of the analytical signal from a univariate calibration (zero order data) to partial least squares (PLS) calibration (first order). The comparison has been done through the figures of merit of the analytical procedure (technique and calibration) in accordance with the ISO norm and the 2002/657/EC European Decision about residuals. 相似文献
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Hollow‐fiber liquid‐phase microextraction for the direct determination of flumequine in urban wastewaters by flow‐injection analysis with terbium‐sensitized chemiluminescence 下载免费PDF全文
Juan Antonio Ocaña‐González María Ramos‐Payán Rut Fernández‐Torres Manuel Callejón‐Mochón Miguel Ángel Bello‐López 《Journal of separation science》2014,37(19):2738-2744
A flow‐injection analysis chemiluminescence method based on the enhancement effect of the flumequine‐Tb(III) complex on the weak native emission of the Ce(IV)‐Na2SO3 system has been developed for the determination of flumequine. The method includes a cleanup and preconcentration stage (750‐fold) of the sample by hollow‐fiber liquid‐phase microextraction using an Accurel® Q 3/2 polypropylene hollow fiber impregnated with 1‐octanol as the supported liquid membrane. The obtained 50 μL acceptor phase was injected in a 1 mM Tb(III) + 4 mM Ce(IV) in 5% v/v H2SO4 stream and mixed with a 2 mM Na2SO3 stream before its introduction into the flow cell. The chemiluminescence signal was linear in the 0.3–15 ng/mL range, with detection and quantitation limits of 0.1 and 0.3 ng/mL, respectively. The method allows the selective extraction and determination of flumequine in wastewater samples, using simpler and lower‐cost instrumentation and with shorter extraction and analysis times than traditional high‐performance liquid chromatography analysis. 相似文献
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Summary A simple rapid method has been developed for the determination of flumequine and oxolinic acid in edible animal tissues. Analytes
are extracted from the sample matrix using dichloromethane in neutral conditions, then back-extracted in 0.01 M sodium hydroxide
and determined by reversed-phase liquid chromatography with fluorimetric detection. The method has been applied to pork, salmon
and chicken muscle with recoveries higher than 77% in all matrices. The detection limits achieved (<1 μg kg−1) allow the determination of these drugs at a residue level far below their MRL Moreover, some variables that may affect the
spiking process have been studied. 相似文献
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D Barrón 《Analytica chimica acta》2003,477(1):21-27
This paper describes capillary electrophoresis (CE) methodology for simultaneous determination of oxolinic acid (OXO) and flumequine (FLU) in spiked chicken tissue using norfloxacin (NOR) as internal standard (IS), with diode array detection. The analytes were extracted using dichlorometane and NaOH and pre-concentrated by solid phase extraction (SPE).The recoveries obtained were 94 and 84% for oxolinic acid and flumequine , respectively. The detection and quantification limits achieved were 15 and 48 μg kg−1 for oxolinic acid, respectively, and 10 and 30 μg kg−1 for flumequine. The sensitivity of the method proposed allows the determination of these drugs at a residue level far below their maximum residue limit (MRL) established by the European Union (EU). 相似文献
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David Perez-GuaitaStéphanie Boudesocque Stéphanie SayenEmmanuel Guillon 《Polyhedron》2011,30(2):438-443
The synthesis of two complexes with the antibiotic flumequine, [Cu(Flumequine)2(OH2)2] (1) and [Zn(Flumequine)2(OH2)2]·H2O (2) is reported. Their molecular structure was elucidated by combining various spectroscopic techniques. The EPR parameters combined with XAS data underline a tetragonal distorted octahedral geometry for the two complexes. The coordination occurs through the carbonyl and carboxylate oxygen atoms in the equatorial plane. The coordination sphere is completed by two water molecules in axial position. 相似文献
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Rodríguez-Díaz RC Fernández-Romero JM Aguilar-Caballos MP Gómez-Hens A 《Analytica chimica acta》2006,578(2):220-226
The potential usefulness of terbium(III) as reagent for the luminescent determination of flumequine residues in food samples has been studied using both fluorescence (FL) and time-resolved (TR) modes and both batch (B) and integrated liquid chromatography (LC)/derivatisation approaches. The system was optimised in each instance to establish the analytical features of the four methods. The dynamic ranges of the calibration graphs, obtained with standard solutions of flumequine, were (ng mL−1): B-FL 0.18-600; B-TR 2.4-150; LC-FL 3.7-1000 and LC-TR 52-3000. The detection limits were also obtained giving the following values (ng mL−1): B-FL 0.055; B-TR 0.7; LC-FL 1.1 and LC-TR 15. The precision, expressed as the percentage of relative standard deviation, was equal or lower than 5.1% in all instances. The LC methods, which avoid the interference of other quinolone antibiotics, were applied to the analysis of chicken muscle and liver, and whole milk samples. The sample pre-treatment only consisted of a deproteinisation step. The validation procedure for the analysis of samples was carried out using EC recommendations, and the decision limit and detection capability were calculated. The recoveries obtained ranged from 95.0% to 103.8%. 相似文献
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