Department of Chemistry, College of Science, Northeast Forestry University, 26 Hexing Road, Harbin 150040, PR China.
Department of Chemistry, College of Science, Northeast Forestry University, 26 Hexing Road, Harbin 150040, PR China.
J Chromatogr A. 2020 Jan 4;1609:460453. doi: 10.1016/j.chroma.2019.460453. Epub 2019 Aug 13.
Mesoporous structured molecularly imprinted polymers combined with restricted access materials (RAM-M-MIPs) were synthesized in this work, then RAM-M-MIPs were used as adsorbents in matrix solid phase dispersion (MSPD) to extract chlorpyrifos residues from soil. The RAM-M-MIPs with mesoporous structure increased adsorptive capacity and accelerated adsorption rate. At the same time, the RAM-M-MIPs with restricted access function showed good exclusion effect toward humic acid in the soil. In addition, the characteristics of RAM-M-MIPs were measured and the optimal experimental conditions of MSPD were explored. In MSPD, the extraction and clean-up procedures can be finished simultaneously, which saved the extraction time. The analyte eluted from soil was determined by LC-MS/MS. The recoveries were in the range of 93.5-106.1% and the relative standard deviations were in the range of 2.8-5.7% at the spiked soil levels of 0.10-10.00 ng g, the detection limit was 0.015 ng g. Based on these analytical validation results, the developed method can be a useful method to determine chlorpyrifos in soil.
本文合成了具有介孔结构的分子印迹聚合物,并将其与限制进入材料(RAM-M-MIPs)结合,然后将 RAM-M-MIPs 用作基质固相分散(MSPD)中的吸附剂,从土壤中提取毒死蜱残留。具有介孔结构的 RAM-M-MIPs 增加了吸附容量并加快了吸附速率。同时,具有限制进入功能的 RAM-M-MIPs 对土壤中的腐殖酸表现出良好的排除效果。此外,还对 RAM-M-MIPs 的特性进行了测量,并探索了 MSPD 的最佳实验条件。在 MSPD 中,提取和净化过程可以同时完成,从而节省了提取时间。从土壤中洗脱的分析物通过 LC-MS/MS 进行测定。在土壤加标水平为 0.10-10.00ng g 时,回收率在 93.5-106.1%范围内,相对标准偏差在 2.8-5.7%范围内,检测限为 0.015ng g。基于这些分析验证结果,所开发的方法可以成为一种有用的方法,用于测定土壤中的毒死蜱。