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机构地区:[1]吉林大学化学学院,长春130012 [2]吉林大学生命科学学院,长春130012
出 处:《分析化学》2016年第4期647-653,共7页Chinese Journal of Analytical Chemistry
基 金:国家自然科学基金(No.21575049);吉林省科技发展计划项目(No.20140101112JC)资助~~
摘 要:以3-(甲基丙烯酸酰氧)丙基三甲氧基硅烷修饰的Fe_3O_4为载体,没食子酸丙酯为模板分子,采用表面印迹技术制备了核壳结构的磁性没食子酸丙酯分子印迹聚合物(Fe_3O_4@SiO _2-MIPS),并将该磁性分子印迹聚合物作为吸附剂引入到微流控芯片中,与HPLC联用,实现对痕量酚类抗氧化剂的分离富集。采用扫描电镜、磁滞回线、热重分析、红外光谱及X射线衍射对该磁性分子印迹聚合物表征。在最佳萃取条件下(样品体积3 mL,样品溶液pH=5.0,样品流速为0.5 mL/min,洗脱液流速为0.3 mL/min),该聚合物对酚类抗氧化剂具有较强的富集作用。3种酚类抗氧化剂在10~5000 ng/mL范围内呈现良好的线性关系,线性相关系数均大于0.9901,日内和日间相对标准偏差(n=5)分别低于2.8%和3.5%。将本方法用于化妆水中酚类抗氧化剂的分析检测,加标回收率在87.9%~104.0%之间,相对标准偏差(n=3)小于3.7%。3-Methacryloxypropyltrimethoxy silane modified Fe_3O_4 was employed as the carrier material to prepare core-shell magnetic molecularly imprinted polymers( Fe_3O_4@ SiO_2-MIPS) by using a surface molecular imprinting technology with propyl gallate as the template. The magnetic composites were loaded into a microchip and coupled with high-performance liquid chromatography to separate and preconcentrate synthetic phenolic antioxidants( SPAs). The structures of the resulting complex were characterized by scanning electron microscopy,vibrating sample magnetoeter,thermogravimetric analysis / differential thermal gravity analysis,Fourier-transformed infrared spectroscopy and X-ray diffraction spectrometry. Under the optimal conditions( 3 mL of sample solution,sample p H of 5. 0,sample flow rate of 0. 5 mL /min,and eluent flow rate of0. 3 mL / min),the magnetic MIPS displayed enhanced adsorption ability for phenolic antioxidants. The calibration curves showed good linearity with correlation coefficients greater than 0. 9901. Intra-day and interday relative standard deviations( RSD) were less than 2. 8% and 3. 5%,respectively. The present method was applied to the determination of phenolic antioxidants in cosmetics samples,illustrating satisfactory recovery( 87. 9%- 104. 0%) and reproducibility( RSD less than 3. 7%).
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