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Abstract
A highly efficient and selective method based on core–shell molecularly imprinted polymers (MIL@MIP) and high performance liquid chromatography (HPLC) was developed and firstly used for the trace analysis of tribenuron-methyl (TBM) in complicated matrices. The MIL@MIP was prepared by surface molecular-imprinting technique, specially using MIL-101 as core, TBM as template molecule, methacrylic acid (MAA) as functional monomer, ethylene glycol dimethacrylate (EGDMA) as cross-linker, and azobisisobutyronitrile (AIBN) as initiator. The resulting MIL@MIP showed high affinity, recognition specificity, fast mass transfer rate, and efficient adsorption performance towards TBM with the adsorption capacity reaching up to 3.217 mg/g. It also showed high cross-selectivity for TBM among its six kinds of chemical structure analogues. Furthermore, using the MIL@MIP as solid-phase extraction (SPE) materials, the recoveries of TBM determined by HPLC were 84.6-92.3%, 93.3-106.7%, and 88.9-93.3% in the spiked river water, soil, and soybean samples, respectively, with the limit of detection of 0.3 ng/L, 1.5 ng/kg, and 1.5 ng/kg, accordingly. It was proved that the developed HPLC-MISPE method was fast, accurate, and sensitive for detecting the trace TBM in river water, soil, and soybean samples.
Highlights
Tribenuron-methyl (TBM) is one of the sulfonylurea herbicides (SUs), which have been widely used to control broadleaved weeds and annual grasses due to their high herbicidal activity, low dosage (4-20g of active ingredient per hectare), and relatively low mammalian toxicity (LD50 > 4000 mg/kg) [1, 2]
Methacrylic acid (MAA), dimethyl formamide (DMF), and toluene were provided by the Guoyao Group Reagent, Co. (Shanghai, China)
It is obvious that MIL-101 was synthesized successfully [35]
Summary
Tribenuron-methyl (TBM) is one of the sulfonylurea herbicides (SUs), which have been widely used to control broadleaved weeds and annual grasses due to their high herbicidal activity, low dosage (4-20g of active ingredient per hectare), and relatively low mammalian toxicity (LD50 > 4000 mg/kg) [1, 2]. Different methods have been developed to determine TBM residues, including high performance liquid chromatography with ultraviolet detector (HPLC-UV) [5], high performance liquid chromatography with mass spectrum (HPLC/MS/MS) [6, 7], capillary electrophoresis (CE) [8,9,10], and enzyme-linked immunoassay (ELISA) [11]. Along with these methods, most sample pretreatments for sulfonylurea analysis used solidphase extraction (SPE) with C18 columns for purification and concentration. A highly selective material and efficient extraction before quantitative determination are essentially necessary
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