scholarly journals Preparation and characterization of molecularly imprinted solid-phase extraction column coupled with high-performance liquid chromatography for selective determination of melamine

2018 ◽  
Vol 5 (9) ◽  
pp. 180750 ◽  
Author(s):  
Q. Zhou ◽  
X. C. Tan ◽  
X. J. Guo ◽  
Y. J. Huang ◽  
H. Y. Zhai

We synthesized a selective molecularly imprinted solid-phase extraction (MIP-SPE) column and established an extraction and enrichment method using this MIP-SPE column. By coupling with HPLC, we developed a new method to detect trace amounts of melamine in eggs. The MIP-SPE column was synthesized by in situ thermal-initiated polymerization using melamine as the template, methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linker and azodiisobutyronitrile as the initiator. HPLC was used to evaluate the identification and enrichment capability of the MIP-SPE column and for the measurement of melamine in the sample. The melamine concentration exhibited an excellent linear relationship in the range of 0.1–25.0 µg ml −1 ( r = 0.9983). The identification capability of the MIP-SPE column was apparently superior to that of the non-imprinted polymer solid-phase extraction column; an average enrichment factor of 46.8-fold (RSD = 3.5%) was obtained for 0.4 µg ml −1 melamine by the MIP-SPE column. When the MIP-SPE HPLC method was applied to the detection of melamine in eggs, an average recovery rate of 93.5–102.0% (RSD = 3.6–4.9%) and a limit of detection of 0.05 µg kg −1 were obtained. This method is simple, fast and cost-effective; thus, it can greatly simplify the pre-treatment of complex samples and can be used in the detection of residual melamine in eggs and other products.

2011 ◽  
Vol 89 (4) ◽  
pp. 517-523 ◽  
Author(s):  
Ke-Jing Huang ◽  
Cong-Hui Han ◽  
Ying-Ying Wu ◽  
Chao-Qun Han ◽  
De-Jun Niu ◽  
...  

A simple and efficient solid-phase extraction – spectrofluorimetric method has been developed to determine glutathione (GSH). Fluorescent probe N-(4,4-difluoro-5,7-dimethyl-4-bora-3a,4a-diaza-s-indacene-3-yl)methyl)iodoacetamide (BODIPY Fl-C1-IA) was used as the derivatization reagent. The procedure was based on a BODIPY Fl-C1-IA selective reaction with GSH to form the highly fluorescent product BODIPY Fl-C1-IA–GSH, using a solid-phase extraction column and spectrofluorimetric determination. The variables affecting analytical performance were studied and optimized. The calibration graph using the preconcentration system for GSH was linear over the range of 1–200 nmol/L with a limit of detection of 0.05 nmol/L (signal-to-noise ratio = 3). The relative standard deviation for six replicate determinations of GSH at the 100 nmol/L concentration level was 3.9%. The method was applied to water samples and average recoveries between 87.5% and 111.5% were obtained for spiked samples.


Author(s):  
Yutaka Gomita ◽  
Katsushi Furuno ◽  
Kohei Eto ◽  
Tamotsu Fukuda ◽  
Yasunori Araki ◽  
...  

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