School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou, 510275, China.
Analyst. 2012 Feb 21;137(4):968-77. doi: 10.1039/c2an16001c. Epub 2011 Dec 20.
In this study, novel GA3 magnetic molecularly imprinted polymer (mag-MIP) beads were synthesized by a microwave irradiation method, and the beads were applied for the trace analysis of gibberellin acids (GAs) in plant samples including rice and cucumber coupled with high performance liquid chromatography-mass spectrometry (HPLC-MS). The microwave synthetic procedure was optimized in detail. In particular, the interaction between GA3 and functional monomers was further studied for the selection of the optimal functional monomers during synthesis. It can be seen that the interaction between GA3 and acrylamide (AM) finally selected was stronger than that between GA3 and other functional monomers. GA3 mag-MIP beads were characterized by a series of physical tests. GA3 mag-MIP beads had a porous and homogeneous surface morphology with stable chemical, thermal and magnetic properties. Moreover, GA3 mag-MIP beads demonstrated selective and specific absorption behavior for the target compounds during unsaturated extraction, which resulted in a higher extraction capacity (∼708.4 pmol for GA3) and selectivity than GA3 mag-non-imprinted polymer beads. Finally, an analytical method of GA3 mag-AM-MIP bead extraction coupled with HPLC-MS detection was established and applied for the determination of trace GA1, GA3, GA4 and GA7 in rice and cucumber samples. It was satisfactory that GA4 could be actually found to be 121.5 ± 1.4 μg kg(-1) in real rice samples by this novel analytical method. The recoveries of spiked rice and cucumber samples were found to be 76.0-109.1% and 79.9-93.6% with RSDs of 2.8-8.8% and 3.1-7.7% (n = 3), respectively. The proposed method is efficient and applicable for the trace analysis of GAs in complicated plant samples.
在这项研究中,通过微波辐射法合成了新型 GA3 磁性分子印迹聚合物(mag-MIP)珠,并将其应用于包括水稻和黄瓜在内的植物样品中痕量分析赤霉素(GAs)与高效液相色谱-质谱(HPLC-MS)联用。详细优化了微波合成程序。特别是,进一步研究了 GA3 和功能单体之间的相互作用,以选择合成过程中的最佳功能单体。可以看出,最终选择的 GA3 和丙烯酰胺(AM)之间的相互作用强于 GA3 和其他功能单体之间的相互作用。通过一系列物理测试对 GA3 mag-MIP 珠进行了表征。GA3 mag-MIP 珠具有多孔且均匀的表面形态,具有稳定的化学、热和磁性能。此外,GA3 mag-MIP 珠在不饱和萃取过程中对目标化合物表现出选择性和特异性吸收行为,导致萃取容量(GA3 约为 708.4 pmol)和选择性高于 GA3 mag-非印迹聚合物珠。最后,建立了一种基于 GA3 mag-AM-MIP 珠萃取结合 HPLC-MS 检测的 GA3 分析方法,并将其应用于测定水稻和黄瓜样品中的痕量 GA1、GA3、GA4 和 GA7。通过这种新型分析方法,令人满意的是,在实际的水稻样品中实际发现 GA4 为 121.5±1.4μgkg(-1)。添加水稻和黄瓜样品的回收率分别为 76.0-109.1%和 79.9-93.6%,相对标准偏差(RSD)为 2.8-8.8%和 3.1-7.7%(n=3)。该方法高效、适用于复杂植物样品中 GAs 的痕量分析。