Microwave synthesis of gibberellin acid 3 magnetic molecularly imprinted polymer beads for the trace analysis of gibberellin acids in plant samples by liquid chromatography-mass spectrometry detection.
Microwave synthesis of gibberellin acid 3 magnetic molecularly imprinted polymer beads for the trace analysis of gibberellin acids in plant samples by liquid chromatography-mass spectrometry detection.
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DOI：
10.1039/c2an16001c
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发表时间：
2012-01
期刊：
影响因子：
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通讯作者：
Zhuomin Zhang;Wei Tan;Yuling Hu;Gongke Li;Song Zan
中科院分区：
文献类型：
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作者：
Zhuomin Zhang;Wei Tan;Yuling Hu;Gongke Li;Song Zan
采用微波辐射法合成了赤霉素3磁性分子印迹聚合物（mag-MIP）微球，并将其应用于水稻和黄瓜等植物样品中赤霉素的痕量分析。对微波合成工艺进行了优化。特别是，GA 3和功能单体之间的相互作用进行了进一步研究，以选择最佳的功能单体在合成过程中。可以看出，GA 3与最终选择的丙烯酰胺（AM）之间的相互作用比GA 3与其他功能单体之间的相互作用更强。通过一系列物理测试表征GA 3 mag-MIP珠。GA 3 mag-MIP微球具有多孔、均匀的表面形貌，并具有稳定的化学、热学和磁学性质。此外，GA 3 mag-MIP珠表现出选择性和特定的吸附行为的目标化合物在不饱和萃取，这导致了更高的萃取容量（708.4 pmol的GA 3）和选择性比GA 3磁非印迹聚合物珠。建立了GA 3 mag-AM-MIP微球萃取-HPLC-MS检测的分析方法，并应用于大米和黄瓜样品中痕量GA 1、GA 3、GA 4和GA 7的测定。结果表明，在真实的大米样品中，GA_4的实际检出量为121.5 ± 1.4 μg·kg ~（-1）。大米和黄瓜样品的加标回收率分别为76.0-109.1%和79.9-93.6%;相对标准偏差分别为2.8-8.8%和3.1-7.7%（n = 3）。该方法适用于复杂植物样品中痕量GAs的分析。
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.