Feng Gege, Sun Jianchun, Wang Miao, Wang Mengqiang, Li Zhuang, Wang Shanshan, Zheng Lufei, Wang Jing, She Yongxin, Abd El-Aty A M
Institute of Quality Standard and Testing Technology for Agro-Products, Chinese Academy of Agricultural Science/Key Laboratory of Agro-Products Quality and Safety of Chinese Ministry of Agriculture, Beijing 100081, P. R. China.
Tibetan Inspection and Testing Center for Agricultural Product Quality and Safety, Lhasa, 850000, P.R. China.
J Chromatogr A. 2021 Jun 21;1647:462143. doi: 10.1016/j.chroma.2021.462143. Epub 2021 Apr 9.
Molecularly imprinting polymers with high selectivity toward 29 sulfonylurea herbicides were synthesized by precipitation polymerization, using metsulfuron-methyl and chlorsulfuron as the template molecule, 4-vinylpyridine as the function monomer, divinylbenzene as the crosslinking agent, and acetonitrile as porogen. The imprinted polymers were characterized and measured by scanning electron microscopy (SEM) and equilibrium adsorption experiments. The molecularly imprinted polymers displayed specific recognition for the tested 29 sulfonylurea herbicides, and the maximum apparent binding capacity was found to be 18.81 mg/g. The synthesized polymer was used as a solid-phase extraction (SPE) column coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for determination of the tested analytes in agro-products. Within the range of 2-100 μg/L, the tested analytes have achieved a good linear association with correlation coefficient (R) > 0.999. The calculated limits of detection (LODs, S/N=3) as along with limits of quantification (LOQs, S/N=10) were in the ranges of 0.005-0.07 μg/L and 0.018-0.23 μg/L, respectively. Under different spiking levels, the recovery rates were ranged from 74.8% - 110.5%, and the relative standard deviation (RSDs) were < 5.3%. Finally, the feasibility of the proposed methodology was successfully applied for detection of sulfonylurea herbicides in crops, vegetables, and oils samples.
以甲磺隆和氯磺隆为模板分子，4-乙烯基吡啶为功能单体，二乙烯基苯为交联剂，乙腈为致孔剂，通过沉淀聚合法合成了对29种磺酰脲类除草剂具有高选择性的分子印迹聚合物。通过扫描电子显微镜（SEM）和平衡吸附实验对印迹聚合物进行了表征和测定。该分子印迹聚合物对所测试的29种磺酰脲类除草剂表现出特异性识别，最大表观结合容量为18.81 mg/g。将合成的聚合物用作固相萃取（SPE）柱，与液相色谱-串联质谱（LC-MS/MS）联用，用于测定农产品中的被测分析物。在2-100 μg/L范围内，被测分析物具有良好的线性关系，相关系数（R）>0.999。计算得到的检测限（LOD，S/N=3）和定量限（LOQ，S/N=10）分别在0.005-0.07 μg/L和0.018-0.23 μg/L范围内。在不同加标水平下，回收率在74.8%-110.5%之间，相对标准偏差（RSD）<5.3%。最后将所提方法成功应用于作物、蔬菜和油类样品中磺酰脲类除草剂的检测。
