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A Biocompatible Solid-Phase Extraction Technique And Its Applications In Food Safety Detection

Posted on:2017-04-22Degree:MasterType:Thesis
Country:ChinaCandidate:L ZhangFull Text:PDF
GTID:2283330503491753Subject:Drug analysis
Abstract/Summary:PDF Full Text Request
Food safety is a major issue related to human health. It requires not only the relevant laws to regulate the production, transportation and marketing of animal-original foods, but also the high efficient techniques for the determination of veterinary residuals. Owing to the complex matrix interferences of animal-original food, it is necessary to develop biocompatible and high-efficient sample pre-treatment technology for veterinary residuals analysis.In this article, two kinds of surfactant-modified solid-phase extraction(SPE) cartridges coupled with high performance liquid chromatography(HPLC) have been developed for the determination of clenbuterol(CLB) in pork samples, respectively. The specific studies are divided into two parts.Objective: The SDS modified SPE column can be used for the direct extraction of CLB from the acidic pork homogenates which can simplified the sample preparation steps.Methods: The SPE Column was dynamically modified with surfactant SDS, and then used for the direct extraction of CLB from the acidic pork homogenates. Finally, these extracts were analyzed by HPLC.Results:The analysis result showed following. Good linearity of CLB ranged from 0.1mg/kg to 10.0mg/kg with correlation coefficient(R2) of0.9989 was obtained. And the average recoveries ranged from 96.36% to103.96% at the three spiked levels with the relative standard deviations(RSD, n=5) from 4.46% to 5.10%. The limit of detection(LOD)come from proteins and other biological macromolecules in pork samples can be effectively reduced in the extraction process.Methods: A certain amount of Tween-20 was loaded onto the ODS SPE column, and then the modified SPE column was used for the extraction of CLB. Finally, these extracts were analyzed by HPLC.Results: Good linearity of CLB ranged from 0.2mg/kg to10.0mg/kg with correlation coefficient(R2) of 0.9986 was obtained. The average recoveries ranged from 96.07% to 107.75% at the three spiked levels of 5.0,1.0, 0.5mg/kg, and the relative standard deviations(RSD, n=5) were 2.27%to 3.51%. The limit of detection(LOD) was25.0μg/kg(S/N=3).Conclusions: The Tween-20 modified SPE column has been successfully used for the extraction of CLB from the pork homogenates.The complex matrix interferences can be reduced effectively due to the size-exclusion mechanism of these hydrophilic surfaces in the modified SPE column. It should be noted that this is a kind of simple and efficient biocompatible solid-phase extraction technology.
Keywords/Search Tags:Biocompatible solid-phase extraction, SDS modified SPE column, Tween-20 modified SPE column, High performance liquid chromatography(HPLC)
PDF Full Text Request
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