超临界流体萃取和高效液相色谱同时测定鸡肉中4种氟喹诺酮类药物残留

建立了一种超临界流体萃取(SFE)-高效液相色谱(HPLC)同时检测鸡肉中4种氟喹诺酮类药物(FQs)的方法。SFE萃取的适宜条件是温度80℃,系统压力为300kg/cm2,总流速为3mL/min,萃取时间为30min,夹带剂甲醇的比率为30%。萃取样品用高效液相色谱荧光检测器(激发光波长290nm,发色光波长455nm)外标法定量。氧氟沙星、诺氟沙星、环丙沙星和恩诺沙星在2.5～50μg/L浓度范围内线性良好,相关系数为0.9876～0.9996,其最低检出限为10～25μg/kg。在25～250μg/kg浓度范围内,平均加标回收率为56.6%～94.2%,相对标准偏差在1.4%～14.1%范围。     

MBR工艺处理诺氟沙星制药废水中污泥龄的影响分析

通过对MBR工艺在处理诺氟沙星制药废水时污泥龄的分析,总结了污泥龄与出水COD、氨氮及m(MLVSS)/m(MLSS)、污泥负荷之间的变化关系。结果表明,污泥龄的最佳运行区间为20～50 d;膜生物反应器中m(MLVSS)/m(MLSS)基本在0.5～0.7;污泥龄与污泥负荷有一定的相关性,污泥龄在20～50 d时,系统运行区间COD污泥负荷为0.12～0.25 kg/(kg·d)。     

诺氟沙星葡萄糖注射液的制备工艺

介绍以诺氟沙星、葡萄糖等为原料生产诺氟沙星葡萄糖注射液的生产工艺,考察了不同生产工艺条件对产品色泽、含量、ｐＨ值等因素的影响。结合现有的生产条件得出了诺氟沙星葡萄糖注射液较为合适的生产工艺条件。     

氟喹诺酮类原料药前景与竞争分析

世界抗感染药物市场重心正由头孢菌素类药物向氟喹诺酮类药物转移 ,氟喹诺酮类药物成为抗生素药物中发展最快的领域。我国氟喹诺酮类原料药的市场前景不仅取决于国际的竞争 ,还在于是否能够把握“重磅炸弹”专利药物过期的契机与同类药物的更迭。氟喹诺酮类原料药企业需要结合自身产品战略 ,分析竞争形势 ,合理调整产品线 ,以获得更强竞争优势。     

Development and validation of an LC–MS/MS/MS method for the quantification of fluoroquinolones in several matrices from treated turkeys

The study presents a sensitive and reliable confirmatory method for the extraction, identification, quantification of five fluoroquinolones (FQ) namely enrofloxacin, ciprofloxacin, difloxacin, sarafloxacin and flumequine, in plasma, liver, kidney, muscle, skin + fat, lung and intestinal content from turkeys.For the extraction and matrix clean-up of FQ residues from all biological matrices, the Quick Easy Cheap Effective Rugged Safe (QuEChERS) methodology was adopted; only for plasma samples acetonitrile was used.The analyses were performed by liquid chromatography with mass spectrometry detection (LC–MS). LC separation was performed on a C18 Kinetex column (100 × 2.1 mm, 2.6 μm, Phenomenex, CA, USA) with gradient elution using ammonium acetate solution (10 mM, pH 2.5) and methanol containing 0.1% formic acid. Mass spectrometric identification was done using an LTQ XL ion trap (Thermo Fisher Scientific, CA, USA), with a heated electrospray ionization probe, in positive ion mode.The method was validated according to the European Legislation (decision 2002/657/EC) and EMA guideline (EMA/CVMP/VICH/463202/2009); selectivity, linearity response, trueness (in terms of recovery), precision (within-day repeatability and within-laboratory reproducibility), limit of detection, limit of quantification, decision limits, detection capability, absolute recovery and robustness were evaluated using turkey blank matrices. All data were within the required limits established for confirmatory methods except for flumequine which presented a recovery value slightly higher than 110% in muscle and intestinal content. For all FQs, all the extraction rates were greater than 70% and limits of quantification ranged from 1.2 μg kg⁻¹ to 118.8 μg kg⁻¹.This fast and robust method was suitable for the identification and quantification of FQ residues in tissues, plasma and intestinal content as confirmed by data obtained from incurred samples of turkeys treated at farm for therapeutic purposes.     

食品中诺氟沙星残留管式化学发光免疫测定法的研究

目的 建立检测食品中诺氟沙星(norfloxacin, NFLX)残留的管式化学发光免疫测定法(chemiluminescence immunoassay, CLIA)。方法 以磁性微粒为固相载体, 通过优化抗原包被浓度、磁微粒稀释度、反应时间及pH值, 建立一种可以检测食品中诺氟沙星残留的管式化学发光免疫测定法。结果 该方法的检测范围为0.1668~68.6804 ng/mL, 检测限为0.1161 ng/mL, 准确度为94.52%, 灵敏度为1.8717 ng/mL, 变异系数<10%, NFLX与洛美沙星、氧氟沙星、恩诺沙星、环丙沙星交叉反应极低。结论 本研究建立的NFLX-CLIA测定法特异性、灵敏度、准确度、重复性均符合要求, 样本前处理简单, 检测时间短, 适用于食品中诺氟沙星残留的检测。     

7-(1-芳磺酰氨基硫代甲酰基哌嗪-4-基)喹诺酮类化合物的合成及其体外抗菌活性

由于氟喹诺酮7-位取代基与该类药物的抗菌谱、生物利用度和不良反应等密切相关,因此对传统氟喹诺酮7-位取代基进行结构修饰是寻找新型氟喹诺酮类抗菌剂的重要途径.鉴于众多芳磺酰硫脲衍生物的抗真菌,抗病毒和抗细菌等广谱生物活性,利用药物设计中的拼合原则,以芳磺酰异硫氰酸醋分别与诺氟沙星和环丙沙星的7位哌嗪基反应,设计合成了10...     

动物性食品中诺氟沙星残留的荧光免疫分析方法研究

利用杂交瘤技术制备了诺氟沙星的单克隆抗体,建立了以抗诺氯沙星单克隆抗体为基础的荧光免疫分析方法,工作曲线表明在10-500μg／L浓度范围内呈良好的线性关系,回归方程为：I=31．9210gC-5．0083,相关系数r=0．9965,对诺氟沙星最低检出限迭6．09μg／L,抑制中浓度为52．88μg／L,且对其它结构类似喹诺酮类药物均有特异性识别。本法可应用于检测动物性食品中残留的微量诺氟沙星。