Institute of Quality Standards and Testing Technology for Agri-Products, Chinese Academy of Agricultural Science, 100081 Beijing, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Aug 1;878(23):2047-53. doi: 10.1016/j.jchromb.2010.05.038. Epub 2010 May 31.
A novel method based on the molecularly imprinted solid-phase extraction (MISPE) procedure has been developed for the simultaneous determination of concentrations of sulfonylurea herbicides such as chlorsulfuron (CS), monosulfuron (MNS), and thifensulfuron methyl (TFM) in maize samples by liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS). The molecularly imprinted polymer (MIP) for sulfonylurea herbicides was synthesized by precipitation polymerization using chlorsulfuron as the template molecule, 2-(diethylamino)ethyl methacrylate (DEAMA) as the functional monomer, and trimethylolpropane trimethacrylate (TRIM) as the cross-linker. The selectivities of the chlorsulfuron template and its analogs on the molecularly imprinted polymer were evaluated by high-performance liquid chromatography (HPLC). The extraction and purification procedures for the solid-phase extraction (SPE) cartridge with a molecularly imprinted polymer as the adsorbent for the selected sulfonylurea herbicides were then established. A molecularly imprinted solid-phase extraction method followed by high-performance liquid chromatography-tandem mass spectrometry for the determination of chlorsulfuron, monosulfuron, and thifensulfuron methyl was also established. The mean recoveries of these compounds in maize were in the range 75-110% and the limits of detection (LOD) of chlorsulfuron, monosulfuron, and thifensulfuron methyl were 0.02, 0.75, and 1.45 microg kg(-1), respectively. It was demonstrated that the MISPE-HPLC-MS/MS method could be applied to the determination of chlorsulfuron, monosulfuron, and thifensulfuron methyl in maize samples.
一种基于分子印迹固相萃取（MISPE）程序的新方法已经被开发出来，用于通过液相色谱-串联四极杆质谱（LC-MS/MS）同时测定玉米样品中磺酰脲类除草剂如氯磺隆（CS）、单磺隆（MNS）和噻吩磺隆甲酯（TFM）的浓度。磺酰脲类除草剂的分子印迹聚合物（MIP）是通过沉淀聚合合成的，以氯磺隆为模板分子，2-（二乙氨基）乙基甲基丙烯酸酯（DEAMA）为功能单体，三羟甲基丙烷三甲基丙烯酸酯（TRIM）为交联剂。通过高效液相色谱（HPLC）评估了氯磺隆模板及其类似物在分子印迹聚合物上的选择性。然后建立了以分子印迹聚合物为吸附剂的固相萃取（SPE）小柱对选定的磺酰脲类除草剂的萃取和净化程序。建立了一种分子印迹固相萃取方法，随后通过高效液相色谱-串联质谱法测定氯磺隆、单磺隆和噻吩磺隆甲酯。这些化合物在玉米中的平均回收率在 75-110%之间，氯磺隆、单磺隆和噻吩磺隆甲酯的检测限（LOD）分别为 0.02、0.75 和 1.45 µg kg(-1)。结果表明，MISPE-HPLC-MS/MS 方法可用于测定玉米样品中的氯磺隆、单磺隆和噻吩磺隆甲酯。
