School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, Liaoning Province 110016, PR China.
School of Pharmaceutical Engineering, Shenyang Pharmaceutical University, Shenyang, Liaoning Province 110016, PR China.
Talanta. 2019 May 1;196:572-578. doi: 10.1016/j.talanta.2018.12.019. Epub 2018 Dec 10.
In this research, microwave assisted magnetic solid phase extraction (MAE-MSPE) coupled with GC-ECD have been successfully used for the determination of eight organochlorine pesticides in soil samples. Specially, the novel FeO-NH@MIL-101(Cr) composites as the MSPE sorbent played a role of selective enrichment and purification towards the targets. The MAE-MSPE procedure was optimized focusing on microwave extraction temperature and time, solution pH, the amount of sorbent, ultrasonic extraction time, ionic strength, elution solvent type, elution solvent volume, and elution time. The parameters of the analytical method were evaluated. Under the optimal condition, the detection limits of α-HCH, β-HCH, γ-HCH, δ-HCH, p,p'-DDE, p,p'-DDD, o,p'-DDT, and p,p'-DDT were in the range of 0.15-0.28 ng g. Satisfactory recoveries were obtained in the range of 71.2-102.4% with the RSDs less than 10.0%. The obtained results demonstrated that the method was suitable for the trace analysis of OCPs. Additionally, molecular docking was employed to calculate the molecular interactions and free binding energies between MIL-101(Cr) and the organochlorines.
在这项研究中,微波辅助磁固相萃取(MAE-MSPE)与 GC-ECD 相结合,成功地用于测定土壤样品中的八种有机氯农药。特别是,新型 FeO-NH@MIL-101(Cr)复合材料作为 MSPE 吸附剂,对目标物具有选择性富集和净化作用。优化了 MAE-MSPE 程序,重点是微波萃取温度和时间、溶液 pH 值、吸附剂用量、超声萃取时间、离子强度、洗脱溶剂类型、洗脱溶剂体积和洗脱时间。评估了分析方法的参数。在最佳条件下,α-HCH、β-HCH、γ-HCH、δ-HCH、p,p'-DDE、p,p'-DDD、o,p'-DDT 和 p,p'-DDT 的检测限在 0.15-0.28 ng g 范围内。回收率在 71.2-102.4%范围内,相对标准偏差(RSD)小于 10.0%。结果表明,该方法适用于痕量分析 OCPs。此外,还采用分子对接计算了 MIL-101(Cr)与有机氯之间的分子相互作用和自由结合能。