Fan Wenying, Gao Mingqi, He Man, Chen Beibei, Hu Bin
Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
Analyst. 2015 Jun 21;140(12):4057-67. doi: 10.1039/c5an00325c. Epub 2015 Apr 15.
In this work, a molecularly imprinted polymer (MIP) coated stir bar was prepared using a self-designed polytetrafluoroethylene (PTFE) mold and in situ polymerization, with cyromazine as the dummy template for the target melamine. The prepared MIP coated stir bar presented a uniform and porous surface as well as good chemical stability and selectivity for melamine. Based on it, a method of MIP coated stir bar sorptive extraction (SBSE) combined with high performance liquid chromatography-ultraviolet detection (HPLC-UV) was developed for the quantification of melamine in food samples. Significant factors affecting the extraction efficiency of melamine by MIP-SBSE, such as the extraction solvent and time, stirring rate, desorption solvent and time, were investigated thoroughly. Under the optimal conditions, the analytical performance of this method was evaluated. The detection limit of the developed method was 0.54 μg L(-1) for melamine with an enrichment factor of 42-fold and the relative standard deviation (RSD) of 6.1% (c = 5 μg L(-1), n = 7), and the linear range was 2-200 μg L(-1). The established method was applied for the determination of melamine in a variety of real samples including cat food, dog food, chicken feed A, chicken feed B and milk powder, and the recoveries for melamine in the spiked samples were in the range of 76.2-98.2%, 80.0-85.5%, 89.5-113%, 85.0-95.5% and 65.0-111%, respectively. The proposed method presented a good specific recognition ability and matrix interference resistance, and was demonstrated to be effective and sensitive for the analysis of melamine in animal food and milk samples.
在本研究中,使用自行设计的聚四氟乙烯(PTFE)模具并通过原位聚合法制备了分子印迹聚合物(MIP)涂层搅拌棒,以环丙氨嗪作为目标三聚氰胺的虚拟模板。制备的MIP涂层搅拌棒表面均匀且多孔,对三聚氰胺具有良好的化学稳定性和选择性。基于此,建立了一种MIP涂层搅拌棒吸附萃取(SBSE)结合高效液相色谱 - 紫外检测(HPLC - UV)的方法用于食品样品中三聚氰胺的定量分析。深入研究了影响MIP - SBSE萃取三聚氰胺效率的重要因素,如萃取溶剂和时间、搅拌速率、解吸溶剂和时间等。在最佳条件下,对该方法的分析性能进行了评估。所建立方法对三聚氰胺的检测限为0.54 μg L⁻¹,富集倍数为42倍,相对标准偏差(RSD)为6.1%(c = 5 μg L⁻¹,n = 7),线性范围为2 - 200 μg L⁻¹。该方法应用于多种实际样品中三聚氰胺的测定,包括猫粮、狗粮、鸡饲料A、鸡饲料B和奶粉,加标样品中三聚氰胺的回收率分别在76.2 - 98.2%、80.0 - 85.5%、89.5 - 113%、85.0 - 95.5%和65.0 - 111%之间。该方法具有良好的特异性识别能力和抗基质干扰能力,被证明对动物食品和牛奶样品中三聚氰胺的分析有效且灵敏。