College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Dec 15;878(32):3421-6. doi: 10.1016/j.jchromb.2010.10.030. Epub 2010 Nov 4.
In this work, a rapid and selective method was successfully developed using the magnetic molecularly imprinted polymer (MMIP) as sorbent for the extraction of β-lactam antibiotics (BLAs) from milk samples. The MMIP has been prepared using penicillin V potassium (PENV) as template molecule, methacrylic acid as functional monomer, ethylene glycol dimethacrylate as crosslinking agent and Fe(3)O(4) magnetite as magnetic component. The experimental results showed that the MMIP had high affinity and selectivity toward PENV and other structurally related BLAs. The extraction process was carried out in a single step by mixing the extraction solvent, MMIPs and milk samples under ultrasonic action. When the extraction was completed, the MMIPs adsorbing the analytes were separated from the sample matrix by an external magnet. The analytes eluted from the MMIP were analyzed by liquid chromatography-tandem mass spectrometry. For achieving optimal preconcentration and reducing non-specific interactions, various parameters affecting the extraction efficiency such as extraction mode, extraction solvent, the amount of MMIPs, extraction time, washing solution and eluting solution were comprehensively evaluated. Under the optimal conditions, the detection limits of BLAs are in the range of 1.6-2.8 ng mL(-1). The relative standard deviations of intra- and inter-day ranging from 3.2% to 8.3% and from 3.6% to 9.8% are obtained, respectively. The method was applied to determine BLAs including PENV, amoxicillin and oxacillin in five milk samples from different provenances. The recoveries of BLAs in these samples from 71.6% to 90.7% are obtained.
在这项工作中，成功开发了一种快速且选择性的方法，该方法使用磁性分子印迹聚合物（MMIP）作为吸附剂从牛奶样品中提取β-内酰胺抗生素（BLAs）。MMIP 是使用青霉素 V 钾（PENV）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。实验结果表明，MMIP 对 PENV 和其他结构相关的 BLAs 具有高亲和力和选择性。通过在超声作用下混合萃取溶剂、MMIP 和牛奶样品，可以一步完成萃取过程。萃取完成后，通过外部磁铁将吸附分析物的 MMIP 从样品基质中分离出来。从 MMIP 洗脱的分析物通过液相色谱-串联质谱进行分析。为了实现最佳的预浓缩并减少非特异性相互作用，综合评估了影响萃取效率的各种参数，如萃取模式、萃取溶剂、MMIP 的量、萃取时间、洗涤溶液和洗脱溶液。在最佳条件下，BLAs 的检测限范围为 1.6-2.8ngmL（-1）。日内和日间相对标准偏差分别为 3.2%-8.3%和 3.6%-9.8%。该方法应用于从不同来源的 5 个牛奶样品中测定包括 PENV、阿莫西林和苯唑西林在内的 BLAs。这些样品中 BLAs 的回收率为 71.6%-90.7%。
