Wenbi Guan

Graphene-dispersive solid-phase extraction of phthalate acid esters from environmental water.

Graphene is a novel carbon nanomaterial with an ultra-high specific surface area. In this paper, we explored graphene as adsorbent for efficient enrichment of 15 phthalate acid esters (PAEs) under different water matrixes (ultrapure water, river and sea). A simple and inexpensive method of dispersive solid-phase extraction (DSPE) combined with gas chromatography-mass spectrometry (GC-MS) was used and acceptable results were provided for most PAEs with overall average recoveries between 71 and 117%. The extraction conditions such as the amount of graphene, the desorption solvent, adsorption time, desorption time and the solution pH were optimized. Finally, the method was applied for the determination of PAEs in environmental water samples including 9 rivers and 2 seas from 7 areas in China.

Amine modified graphene as reversed-dispersive solid phase extraction materials combined with liquid chromatography-tandem mass spectrometry for pesticide multi-residue analysis in oil crops.

Amine modified graphene is successfully synthesized via a one-pot solvothermal reaction between graphene oxide and ammonia water, methylamine or n-butyl amine. The presence of amine groups in graphene is identified by Fourier-transform infrared spectrometry, X-ray photoelectron spectroscopy and an X-ray diffractometer. The ability of amine modified graphene to cleanup fatty acids and other interfering substances from acetonitrile extracts of oil crops has been evaluated. It is found that the resulting CH3NH-G exhibits the best performance in interfering substances removal. Meanwhile, a multi-residue method is validated on 28 representative pesticide residues in four oil crops (rapeseed, peanut, sesame seeds and soybean). This method is based on modified QuEChERS sample preparation with CH3NH-G as reversed-dispersive solid phase extraction material and liquid chromatography-tandem mass spectrometry. Use of matrix-matched standards provides acceptable results for most pesticides with overall average recoveries between 70.5 and 100% and consistent RSDs<13%, except for pymetrozine, thidiazuron and diuron. In any case, this method still meets the 0.1-8.3 μg/kg detection limit needs for most pesticides and may be used for qualitative screening applications, in which any identified pesticides can be quantified and confirmed by a more intensive method that achieves >70% recovery.

Graphene as dispersive solidphase extraction materials for pesticides LC-MS/MS multi-residue analysis in leek, onion and garlic

A multi-residue analytical method was validated for 24 representative pesticides residues in onion, garlic and leek. The method is based on modified QuEChERS sample preparation with a mixture of graphene, primary secondary amine (PSA), and graphitised carbon black (GCB) as reversed-dispersive solid-phase extraction (r-DSPE) material and LC-MS/MS. Graphene was first used as an r-DSPE clean-up sorbent in onion, garlic and leek. The results first show that the mixed sorbent of graphene, PSA and GCB has a remarkable ability to clean-up interfering substances in the r-DSPE procedure when compared with the mixture of PSA and GCB. Use of matrix-matched standards provided acceptable results for tested pesticides with overall average recoveries between 70.1% and 109.7% and consistent RSDs <15.6%. In any case, this method still meets the 1–10 μg kg–1 detection limit needed for pesticide testing and may be used for qualitative screening applications in which any identified pesticides can be quantified and confirmed by a more intensive method that achieves >70% recovery. Graphical Abstract

Residues and dissipation dynamics of molluscicide metaldehyde in cabbage and soil.

The dissipation of metaldehyde on cabbage and in soil was studied and half-life (DT(50)) was estimated in a field study carried out at three different locations. Metaldehyde was sprayed on cabbage at 937.5 and 1406.25 ga.i.ha(-1) for residue study and 1,875 ga.i.ha(-1) for dissipation study in cabbage and soil. Samples of cabbage and soil for dissipation experiment were collected at 0, 1, 2, 3, 5, 7, 14 and 21 days after treatment. For residue studies, cabbage and soil samples were sampled at 5, 7 and 10 days after treatment. Quantification of residues was done by LC-MS/MS. The DT(50) of metaldehyde in cabbage and soil were 0.48-1.61 days and 0.75-1.02 days, respectively, when applied at 2 times of the recommended high dosage. Residues of metaldehyde in cabbage were all below the maximum residue levels of 1.0 mg kg(-1) at both recommended high dosage and 1.5 times the recommended high dosage.

Residues and dissipation of guadipyr in rice ecological system

A modified QuEChERs method with liquid chromatography-tandem mass spectrometry for analysis of guadipyr residue and dissipation in rice matrices, paddy soil and paddy water was developed and validated. Mean recoveries and relative standard deviations in paddy soil, paddy water, rice plant, rice straw, rice hull and husked rice matrices at three spiking levels were 83.1–116.5% and 1.6–9.5%, respectively. The half-life of guadipyr was determined in 2 years at three different field sites in China via a dissipation experiment. The half-lives of guadipyr in paddy water were 0.22–0.37 days, 0.24–3.33 days in paddy soil and 0.44–1.90 days in rice plant. The terminal residues of guadipyr ranged from ND (concentrations of guadipyr were below limit of detection) to 50 μg kg−1 in paddy soil, 10–470 μg kg−1 in rice hull, ND70 μg kg−1 in husked rice and ND to 110 μg kg−1 in rice straw. The results would be helpful in fixing maximum residue limit of guadipyr, a new insecticide, in rice.