College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012, Jilin, China.
Anal Chim Acta. 2010 Mar 3;662(1):31-8. doi: 10.1016/j.aca.2010.01.001. Epub 2010 Jan 11.
A simple method based on magnetic separation for selective extraction of fluoroquinolones (FQs) from environmental water samples has been developed using magnetic molecularly imprinted polymer (MMIP) as sorbent. The MMIP has been prepared using ciprofloxacin as template molecule, methacrylic acid as functional monomer, ethylene glycol dimethacrylate as cross-linking agent and Fe(3)O(4) magnetite as magnetic component. The polymer has been characterized by scanning electron microscopy, Fourier-transform infrared spectrometry and vibrating sample magnetometry. Various parameters affecting the extraction efficiency were evaluated in order to achieve optimal concentration and reduce non-specific interactions. The analytes desorbed from the polymers were determined by liquid chromatography-tandem mass spectrometry. The matrix effect was evaluated by using different washing solvents for removing interfering compounds from the MMIPs after sample loading. Under the optimal conditions, the linearity of the method obtained is in the range of 20-2000 ng L(-1). The detection limits of FQs are in the range of 3.2-6.2 ng L(-1). The relative standard deviations of intra- and inter-day tests ranging from 2.5 to 7.2% and from 3.6 to 9.1% are obtained. In all three spiked levels (20, 100 and 200 ng L(-1)), the recoveries of FQs are in the range of 76.3-94.2%. The proposed method was successfully applied to determine FQs including ciprofloxacin, enrofloxacin, lomefloxacin, levofloxacin, fleroxacin and sparfloxacin in different water samples, such as lake water, river water, primary and final sewage effluent. Ciprofloxacin and fleroxacin were found in primary and final sewage effluent samples with the contents in the range of 26-87 ng L(-1).
一种基于磁分离的从环境水样中选择性提取氟喹诺酮类(FQs)的简单方法已经使用磁性分子印迹聚合物(MMIP)作为吸附剂开发出来。MMIP 是使用环丙沙星作为模板分子、甲基丙烯酸作为功能单体、乙二醇二甲基丙烯酸酯作为交联剂和 Fe(3)O(4)磁铁矿作为磁性成分制备的。通过扫描电子显微镜、傅里叶变换红外光谱和振动样品磁强计对聚合物进行了表征。为了达到最佳的浓度并减少非特异性相互作用,评估了影响萃取效率的各种参数。从聚合物中解吸的分析物通过液相色谱-串联质谱法进行测定。通过使用不同的洗涤溶剂来评估基质效应,以便在样品加载后从 MMIP 中去除干扰化合物。在最佳条件下,该方法的线性范围为 20-2000ngL(-1)。FQs 的检测限范围为 3.2-6.2ngL(-1)。日内和日间测试的相对标准偏差分别为 2.5-7.2%和 3.6-9.1%。在三个加标水平(20、100 和 200ngL(-1))下,FQs 的回收率范围为 76.3-94.2%。该方法成功应用于测定不同水样中的氟喹诺酮类,包括环丙沙星、恩诺沙星、洛美沙星、左氧氟沙星、氟罗沙星和司帕沙星,如湖水、河水、原水和最终污水。在原水和最终污水样品中发现了环丙沙星和氟罗沙星,含量在 26-87ngL(-1)范围内。