大孔聚合物整体柱吸管的制备及其从人血清和尿液中固相萃取柯诺辛碱的应用

Preparation of Macroporous Polymer Monolithic Column Tip and Its Application to the Extraction of Corynoxine in Human Serum and Urine

以甲基丙烯酸和甲基丙烯酸丁酯为功能单体,乙二醇二甲基丙烯酸酯为交联剂,超高分子量的多分散二醋酸纤维素作为致孔剂,在1000μL移液器吸管中制备聚合物整体柱,并将其应用于从人血清和尿液中萃取柯诺辛碱。整体柱截面的扫描电子显微图显示,柱体内存在大的微米级通孔,从图上测量最大的接近10μm。大的通孔确保了整体柱具有良好流通性,该整体柱吸管可以安装于移液器上,通过手动操作,快速完成对生理体液样品的固相萃取操作。将整体柱吸管与高效液相色谱联合,成功应用于检测人血清和尿液中的柯诺辛碱。结果表明血清样品在5.44～152μg/m L范围内线性关系良好,R2为0.9993,血清质控样品检测的RSD%在2.4%～10%之间,相对回收率为92.5%～105%,绝对回收率为81.5%～91.1%;尿液样品在5.21～130.9μg/m L范围内线性关系良好,R2为0.9991,质控样品检测RSD%为1.3%～6.3%,相对回收率为86.0%～110%,绝对回收率为90.3～101%。本方法可以简单、快速、准确的检测人血清和尿液中的柯诺辛碱含量。

Using methacrylic acid and butyl methacrylate as functional monomers, ethylene glycol dimethacrylate as cross-linking agent, ultra-high molecular weight polydisperse cellulose diacetate as porogen to prepare polymer monolithic column in 1000μ L pipette tip. The section of monolithic column was characterized by scanning electron microscopy(. The results showed that there are macropores at micrometer level(the largest size of macropore near 10 micrometer was observed from the SEM figures.). These macropores ensure the good permeability in the monolithic column which can be connected to a hand held pipettor quickly to perform solid phase extraction. High performance liquid chromatography coupled with tip-SPE method has been established and validated with the spiked human serum and urine samples. A good linear relationship over the range of 5.44~152 μg/m L was observed for human serum(R2 0.9993) with RSD% between 2.4 %~10 % the relative recovery rate between 92.5 %~105 %, and the absolute recovery between 82.6 %~91.1 %. A good linear relationship over the range of 5.21~130.9 μg/m L was observed for human urine(R2 0.9991) with the RSD% between 1.3 %~6.3 %, the relative recovery rate between 86.0 %~110 %, and the absolute recovery rate between 90.3 %~101 %. The method can be used to quickly and accurately detect the content of corynoxine in human serum and urine.