Faculty of Chemistry, Shahid Beheshti University, G. C., P.O. Box 1983963113, Evin, Tehran, Islamic Republic of Iran.
Mikrochim Acta. 2020 Mar 9;187(4):209. doi: 10.1007/s00604-020-4174-2.
A new ultrasonic-assisted dispersive solid-phase extraction method using mesoporous nanosorbent composed of silica, graphene, and palladium (II) (M S/G@-SH@Pd (II)), coupled with corona discharge ion mobility spectrometry, was developed for trace determination of organophosphorus pesticides. Initially, the M S/G@-SH@Pd (II) nanosorbent was synthesized and characterized. Then, the nanosorbent was used for the sorption and extraction of organophosphorus pesticides. Under the optimized conditions (pH = 7.0, 15 mg of sorbent, 3 min extraction time, ethanol as desorption agent, 3 min centrifuge time), the proposed technique provided good linearity (R > 0.994), repeatability (RSD < 4.6%), low limits of detection (0.15-0.30 ng mL), excellent preconcentration factor (PF = 472-478), and high recoveries (93-94%). The method was applied to the determination of organophosphorus pesticides in real water samples. The sorbent was reused in 5 cycles without any considerable loss of activity. Graphical abstract Schematic presentation of design and synthesis of mesoporous nanosorbent composed of silica, graphene, and palladium (II) for ultrasound-assisted dispersive solid-phase extraction of organophosphorus pesticides prior to their quantitation by ion mobility spectrometry.
一种新的超声辅助分散固相萃取方法,使用由二氧化硅、石墨烯和钯(II)组成的中孔纳米吸附剂(M S/G@-SH@Pd (II)),与电晕放电离子淌度谱联用,用于痕量测定有机磷农药。首先合成并表征了 M S/G@-SH@Pd (II)纳米吸附剂。然后,纳米吸附剂用于有机磷农药的吸附和萃取。在优化条件下(pH=7.0,15 mg 吸附剂,3 min 萃取时间,乙醇作为洗脱剂,3 min 离心时间),提出的技术提供了良好的线性(R>0.994)、重复性(RSD<4.6%)、低检测限(0.15-0.30 ng mL)、出色的浓缩因子(PF=472-478)和高回收率(93-94%)。该方法应用于实际水样中有机磷农药的测定。吸附剂在没有明显活性损失的情况下可重复使用 5 次。