Xue Liu

Pesticide Multi-Residue Analysis in Tea Using d-SPE Sample Cleanup with Graphene Mixed with Primary Secondary Amine and Graphitized Carbon Black Prior to LC–MS/MS

Graphene is a novel class of carbon nanostructures with ultrahigh specific surface area. Graphene has already been used in many fields and has great promise for use in sorbent materials. In this study, we used graphene mixed with primary secondary amine (PSA) and graphitized carbon black (GCB) as dispersive solid-phase extraction materials for the cleanup of tea for the first time. Compared to the literature, the amount of PSA and GCB was greatly reduced. A multi-residue method combined with liquid chromatography–tandem mass spectrometry was validated for rapid determination of 25 pesticide residues in tea. Green tea, black tea, and white tea were selected as matrixes, representing the majority of tea types. Recoveries ranged from 71.1 to 108.3xa0% and consistent relative standard deviations <13.6xa0% for all 25 pesticides. Graphene has significant potential as a promising new adsorbent for pesticide residue analysis of teas. This method can be used to analyze tea samples with different degrees of fermentation.

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

Evaluation of Graphene for Effective Cleanup of Fruit and Vegetable Extracts in Pesticide Residue Analysis

Graphene is a novel class of carbon nanostructures which possess an ultra-high specific surface area. It has already been used for pre-concentration, extraction, and electrochemical selective determination of pesticides but not much work has been focused on the cleanup efficiency of graphene. In this work, graphene was evaluated as an alternative cleanup sorbent for gas chromatography-mass spectrometry (GC-MS) analysis of 17 pesticides analyzed in vegetables and fruit with the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method. QuEChERS is a standard method published by CEN (European Committee for Standardization) Code EN 15662: 2008. The recoveries of the 17 pesticides in carrot, grape, tomato and rape were 92–120xa0% with relative standard deviations below 10xa0%. Comparative studies showed that graphene not only has good removal efficiencies of pigments in vegetables and fruit, but also has better cleanup ability than commonly used graphitized carbon black (GCB).

Synthesis of TiO2–Reduced Graphene Oxide Nanocomposites for Efficient Adsorption and Photodegradation of Herbicides

The elimination of herbicides in aquatic environment is influenced by various biotic or abiotic factors. Thus, efficient, more applicable, and flexible methods are in demand. Photodegradation has been applied to remove three main types of herbicides, phenylurea, triazine, and chloroacetanilide, from water, based on a series of TiO2–reduced graphene oxide nanocomposites. Experimental results showed that the three types of herbicides could be mostly removed under simulated sunlight irradiation for 5xa0h with the as-prepared photocatalyst. Compared with pure TiO2 or P25, the photodegradation efficiency has been markedly increased. Thus, the present work could promote a new strategy dealing with the pollution of herbicides in aquatic ecosystems.

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.

Correction to Photodegradation of Imidacloprid in Aqueous Solution by the Metal-Free Catalyst Graphitic Carbon Nitride using an Energy-Saving Lamp

Imidacloprid has become a research hotspot, due to its high toxicity to bees and other nontarget organisms. Photodegradation is a common method for removing imidacloprid in an aquatic environment. Traditional methods of pesticide photodegradation have generally been confined by many factors, such as response to only high-energy ultraviolet light. Herein, the visible-light-driven photocatalyst graphitic carbon nitride (g-C3N4) was applied to the photodegradation of imidacloprid. Visible-light illumination (λ >400 nm) resulted in nearly 90% substrate transformation in 5 h. With the illumination of an energy-saving lamp, imidacloprid has also been mostly removed. 1-((6-chloropyridin-3-yl)methylhydroxy)imidazolidin-2-ylidene nitramide) and 4,5-dihydro-N-nitro-1-(3-pyridinylmethyl)-1H-imidazol-2-amine were the main photoproducts identified by LC-MS analysis. The photocatalytic mechanism has also been discussed. This work could provide new perspective that g-C3N4, as a good visible-light photocatalyst could be ...

A carbonised sieve-like corn straw cellulose–graphene oxide composite for organophosphorus pesticide removal

The development of efficient adsorbents for the removal of organophosphorus pesticides from water is a major challenge. In this work, we prepared an activated carbon derived from sieve-like cellulose/graphene oxide composites (ACCE/G) for the removal of several organophosphorus pesticides. We employed corn straw to produce a sieve-like cellulose–graphene oxide composite (CCE/G); then, by treating CCE/G with potassium hydroxide at high temperatures, the efficient adsorbent ACCE/G was prepared. The adsorption capacity of ACCE/G is higher than those of other sorbents, including a multi-wall carbon nanotube, graphitised carbon black, activated carbon, C18, and primary secondary amine adsorbent. The ACCE/G structure has been fully characterised via scanning electron microscopy, Fourier-transform infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction and Brunauer–Emmett–Teller analysis. The maximum adsorption capacity of ACCE/G is 152.5 mg g−1 for chlorpyrifos. The mechanism, the thermodynamic properties, and the kinetics of the adsorption process have been investigated as well. Our findings demonstrate that the adsorption mechanism depends on the electron-donating abilities of the S and P atoms. Moreover, the Langmuir model gives the best fit for the isotherm data, and the adsorption efficiency of the ACCE/G is still over 80% after eight times of recycling, making ACCE/G a valuable candidate for the removal of OPPs.

Rapid adsorption and enhanced removal of emodin and physcion by nano zirconium carbide.

In this study, nano zirconium carbide (n-ZrC) was synthesized by preceramic polymers method, and it was used to adsorb emodin and physcion from solutions for the first time. The prepared material was characterized by various technologies. The adsorption experiment was carried out to investigate the emodin and physcion removal performance. The results indicate that the pseudo-second-order kinetic model and the Langmuir model correlated satisfactorily to the experimental data, and the thermodynamic parameters are also calculated. Especially, n-ZrC can remove >95% of emodin or physcion in a minute under the optimal conditions, it is the fastest adsorption rate compared to other commonly used adsorbents (commercial zirconium carbide, activated carbon, C18, PSA, GCB and florisil). The adsorption mechanism was discussed, which suggests that Van der Waals forces are the primary driving power during the adsorption process. Moreover, n-ZrC is stable at different pH and it can be reused at least fifteen times.

Mesoporous activated carbon from starch for superior rapid pesticides removal

Pesticides contamination of water has caused considerable concern due to the potential hazard to human health. For the first time, mesoporous activated carbon from starch (ACS) was applied to remove pesticides from water. ACS could remove 11 pesticides rapidly (shake five times). The adsorption rates of ACS (>80%) for the 11 pesticides were higher than those of other adsorbents, including commercial activated carbon (AC), graphitised carbon black (GCB), C18, and primary secondary amine adsorbent (PSA). The mechanisms of the adsorption process for pyraclostrobin were also investigated. The pseudo-second-order model could better describe the adsorption for pyraclostrobin (R2u202f=u202f0.99950). Langmuir model gave the best fit for the isotherm data (R2u202f=u202f0.99899). Our findings demonstrate that oxygen-containing functional groups, N atom and π-bonding network of benzene promoted the adsorption. The adsorption efficiency of the ACS for 11 pesticides was still over 80% after five cycles.