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Rapid and selective determination of melamine from eggs and milk based on magnetic surface molecularly imprinting technology†
Analytical Methods ( IF 2.7 ) Pub Date : 2017-11-21 00:00:00 , DOI: 10.1039/c7ay02055d Li Wang 1, 2, 3, 4 , Fen Qiu 1, 2, 3, 4 , Jian Li 1, 2, 3, 4 , Jiarong Pan 1, 2, 3, 4
Analytical Methods ( IF 2.7 ) Pub Date : 2017-11-21 00:00:00 , DOI: 10.1039/c7ay02055d Li Wang 1, 2, 3, 4 , Fen Qiu 1, 2, 3, 4 , Jian Li 1, 2, 3, 4 , Jiarong Pan 1, 2, 3, 4
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In this study, a rapid and selective method based on magnetic surface molecularly imprinting technology coupled with high performance liquid chromatography was used for the determination of melamine from egg and milk samples. A novel magnetic surface molecularly imprinted polymer (Fe3O4@SiO2@MIPs) with super-paramagnetic properties and high selectivity for melamine was synthesized as a magnetic adsorbent. The extraction, purification, and concentration processes were carried out simultaneously in a single step using an external magnet. The Fe3O4@SiO2@MIPs were characterized by scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). The adsorption thermodynamics, kinetics, and selectivity were used to investigate the rebinding mechanism of the proposed polymers, which showed better affinity and selectivity as compared to Fe3O4@SiO2@NIPs. In addition, the matrix effect was evaluated. Various parameters, such as extraction solvent, pH of the solution, amount of the polymers, extraction time, washing conditions, and eluent, affecting the extraction efficiency were evaluated. The calibration curves show a satisfactory linear relationship (r = 0.9990–0.9997) in the linear range of 0.1–1000 ng g−1. The limit of detection (LOD) was 0.79 ng g−1 for milk and 0.43 ng g−1 for eggs. Recoveries ranging from 88.4 to 98.2% were obtained with the intra- and inter-day RSDs in the range of 3.5–5.4% and 5.7–7.8%, respectively. The proposed Fe3O4@SiO2@MIPs were successfully applied towards the selective determination of melamine in different real egg and milk samples, and satisfactory recoveries in the range from 87.9% to 102.4% with an RSD of less than 5.40% were obtained. The proposed method simplified the procedures of the classical solid-phase extraction (SPE) method and improved the reliability of the applied method.
中文翻译：
基于磁性表面分子印迹技术快速，选择性地测定鸡蛋和牛奶中的三聚氰胺†
在这项研究中，基于磁性表面分子印迹技术和高效液相色谱法的快速，选择性方法用于测定鸡蛋和牛奶样品中的三聚氰胺。合成了具有超顺磁性和对三聚氰胺具有高选择性的新型磁性表面分子印迹聚合物（Fe 3 O 4 @SiO 2 @MIPs）作为磁性吸附剂。使用外部磁体在单个步骤中同时进行提取，纯化和浓缩过程。Fe 3 O 4 @SiO 2通过扫描电子显微镜（SEM）和振动样品磁力计（VSM）对@MIP进行表征。用吸附热力学，动力学和选择性研究了所提出的聚合物的再结合机理，与Fe 3 O 4 @SiO 2 @NIPs相比，它具有更好的亲和力和选择性。另外，评估了基质效应。评估了影响萃取效率的各种参数，例如萃取溶剂，溶液的pH值，聚合物的量，萃取时间，洗涤条件和洗脱液。在0.1–1000 ng g -1的线性范围内，校准曲线显示出令人满意的线性关系（r = 0.9990–0.9997）。检出限（LOD）为0.79 ng g-1用于牛奶和0.43纳克克-1鸡蛋。日内和日间RSD分别在3.5–5.4％和5.7–7.8％的范围内，回收率介于88.4％至98.2％之间。所提出的Fe 3 O 4 @SiO 2 @MIPs已成功用于不同鸡蛋和牛奶样品中三聚氰胺的选择性测定，回收率在87.9％至102.4％之间，相对标准偏差小于5.40％。 。该方法简化了经典固相萃取（SPE）方法的流程，并提高了所应用方法的可靠性。
更新日期：2017-11-21
中文翻译：
基于磁性表面分子印迹技术快速，选择性地测定鸡蛋和牛奶中的三聚氰胺†
在这项研究中，基于磁性表面分子印迹技术和高效液相色谱法的快速，选择性方法用于测定鸡蛋和牛奶样品中的三聚氰胺。合成了具有超顺磁性和对三聚氰胺具有高选择性的新型磁性表面分子印迹聚合物（Fe 3 O 4 @SiO 2 @MIPs）作为磁性吸附剂。使用外部磁体在单个步骤中同时进行提取，纯化和浓缩过程。Fe 3 O 4 @SiO 2通过扫描电子显微镜（SEM）和振动样品磁力计（VSM）对@MIP进行表征。用吸附热力学，动力学和选择性研究了所提出的聚合物的再结合机理，与Fe 3 O 4 @SiO 2 @NIPs相比，它具有更好的亲和力和选择性。另外，评估了基质效应。评估了影响萃取效率的各种参数，例如萃取溶剂，溶液的pH值，聚合物的量，萃取时间，洗涤条件和洗脱液。在0.1–1000 ng g -1的线性范围内，校准曲线显示出令人满意的线性关系（r = 0.9990–0.9997）。检出限（LOD）为0.79 ng g-1用于牛奶和0.43纳克克-1鸡蛋。日内和日间RSD分别在3.5–5.4％和5.7–7.8％的范围内，回收率介于88.4％至98.2％之间。所提出的Fe 3 O 4 @SiO 2 @MIPs已成功用于不同鸡蛋和牛奶样品中三聚氰胺的选择性测定，回收率在87.9％至102.4％之间，相对标准偏差小于5.40％。 。该方法简化了经典固相萃取（SPE）方法的流程，并提高了所应用方法的可靠性。
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