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      Comparison of Sin-QuEChERS Nano and d-SPE Methods for Pesticide Multi-Residues in Lettuce and Chinese Chives

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          Abstract

          In this study, a new rapid cleanup method was developed for the analysis of 111 pesticide multi-residues in lettuce and Chinese chives by GC–MS/MS and LC–MS/MS. QuEChERS (quick, easy, cheap, effective, rugged and safe)-based sample extraction was used to obtain the extracts, and the cleanup procedure was carried out using a Sin-QuEChERS nano cartridge. Comparison of the cleanup effects, limits of quantification and limits of detection, recoveries, precision and matrix effects (MEs) between the Sin-QuEChERS nano method and the classical dispersive solid phase extraction (d-SPE) method were performed. When spiked at 10 and 100 μg/kg, the number of pesticides with recoveries between 90% to 110% and relative standard deviations < 15% were greater when using the Sin-QuEChERS nano method. The MEs of Sin-QuEChERS nano and d-SPE methods ranged between 0.72 to 3.41 and 0.63 to 3.56, respectively. The results verified that the Sin-QuEChERS nano method was significantly more effective at removing pigments and more convenient than the d-SPE method. The developed method with the Sin-QuEChERS nano cleanup procedure was applied successfully to determine pesticide residues in market samples.

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          Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables.

          This article describes the comparison of different versions of an easy, rapid and low-cost sample preparation approach for the determination of pesticide residues in fruits and vegetables by concurrent use of gas and liquid chromatography (GC and LC) coupled to mass spectrometry (MS) for detection. The sample preparation approach is known as QuEChERS, which stands for "quick, easy, cheap, effective, rugged and safe". The three compared versions were based on the original unbuffered method, which was first published in 2003, and two interlaboratory validated versions: AOAC Official Method 2007.01, which uses acetate buffering, and European Committee for Standardization (CEN) Standard Method EN 15662, which calls for citrate buffering. LC-MS/MS and GC-MS analyses using each method were tested from 50 to 1000ng/g in apple-blueberry sauce, peas and limes spiked with 32 representative pesticides. As expected, the results were excellent (overall average of 98% recoveries with 10% RSD) using all 3 versions, except the unbuffered method gave somewhat lower recoveries for the few pH-dependent pesticides. The different methods worked equally well for all matrices tested with equivalent amounts of matrix co-extractives measured, matrix effects on quantification and chemical noise from matrix in the chromatographic backgrounds. The acetate-buffered version gave higher and more consistent recoveries for pymetrozine than the other versions in all 3 matrices and for thiabendazole in limes. None of the versions consistently worked well for chlorothalonil, folpet or tolylfluanid in peas, but the acetate-buffered method gave better results for screening of those pesticides. Also, due to the recent shortage in acetonitrile (MeCN), ethyl acetate (EtOAc) was evaluated as a substitute solvent in the acetate-buffered QuEChERS version, but it generally led to less clean extracts and lower recoveries of pymetrozine, thiabendazole, acephate, methamidophos, omethoate and dimethoate. In summary, the acetate-buffered version of QuEChERS using MeCN exhibited advantages compared to the other tested methods in the study. Published by Elsevier B.V.
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            Determination of carbamate residues in fruits and vegetables by matrix solid-phase dispersion and liquid chromatography-mass spectrometry.

            Thirteen carbamates were analysed in orange, grape, onion and tomatoes by matrix solid-phase dispersion (MSPD) followed by liquid chromatography-mass spectrometry (LC-MS). Electrospray (ES) and atmospheric pressure chemical ionisation (APCI) were compared and both gave similar results in terms of sensitivity and structural information because at 20 V fragmentor voltages the fragmentation is minimal. The efficiency of different solid-phases (C18, C8, cyano, amine and phenyl) for the MSPD was compared. Mean recoveries using C8 varied from 64 to 106% with relative standard deviations of 5-15% in the concentration range of 0.01-10 mg kg(-1). Matrix constituents did not interfere significantly with the ionisation process of carbamates. The limits of detection were typically in the 0.001-0.01 mg kg(-1) range, which were between 10 and 100 times lower than the maximum residue levels (MRLs) established by the European Union (EU). The method was applied to residue detection in fruit and vegetable samples taken from Valencian markets, in which carbamates were detected at low concentrations.
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              Multi-walled carbon nanotubes as alternative reversed-dispersive solid phase extraction materials in pesticide multi-residue analysis with QuEChERS method.

              A multi-residue method based on modified QuEChERS sample preparation with multi-walled carbon nanotubes (MWCNTs) as reversed-dispersive solid phase extraction (r-DSPE) material and gas chromatography-mass spectrometry determination by selected ion monitoring (GC/MS-SIM) mode was validated on 30 representative pesticides residues in vegetables and fruits. The acetonitrile-based QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation technique was used to obtain the extracts, and the further cleanup was carried out by applying r-DSPE. It was found that the amount of MWCNTs influenced the cleanup performance and the recoveries. The optimal amount of 10mg MWCNTs was suitable for cleaning up all selected matrices, as a suitable alternative r-DSPE material to primary secondary amine (PSA). This method was validated on cabbage, spinach, grape and orange spiked at concentration levels of 0.02 and 0.2 mg/kg. The recoveries of 30 pesticides were in the range of 71-110%, with relative standard deviations (RSDs, n=5) lower than 15%. Matrix effects were observed by comparing the slope of matrix-matched standard calibration with that of solvent. Good linearity was achieved at the concentration levels of 0.02-0.5 mg/L. The limits of quantification (LOQs) and the limits of detection (LODs) for 30 pesticides ranged from 0.003 to 0.05 mg/kg and 0.001 to 0.02 mg/kg at the signal-to-noise ratio (S/N) of 10 and 3, respectively. The method was successfully applied to analysis real samples in Beijing. In conclusion, the modified QuEChERS method with MWCNTs cleanup step showed reliable method validation performances and good cleanup effects in this study. Copyright © 2011 Elsevier B.V. All rights reserved.
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                Author and article information

                Journal
                Molecules
                Molecules
                molecules
                Molecules
                MDPI
                1420-3049
                27 July 2020
                August 2020
                : 25
                : 15
                : 3391
                Affiliations
                [1 ]Institute of Quality and Standard for Agro-Products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China; gqblyj@ 123456163.com (Y.L.); cpzhang1215@ 123456126.com (C.Z.)
                [2 ]Department of Applied Chemistry, College of Science, China Agricultural University, Beijing 100193, China; anquanshun@ 123456cau.edu.cn
                Author notes
                [* ]Correspondence: panc@ 123456cau.edu.cn (C.P.); zhangzh@ 123456mail.zaas.ac.cn (Z.Z.); Tel.: +86-10-62731978 (C.P.); +86-571-86419053 (Z.Z.)
                Author information
                https://orcid.org/0000-0002-7417-0630
                Article
                molecules-25-03391
                10.3390/molecules25153391
                7435897
                32726966
                af6e4212-e921-4c09-993e-e845a85fc351
                © 2020 by the authors.

                Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license ( http://creativecommons.org/licenses/by/4.0/).

                History
                : 28 June 2020
                : 22 July 2020
                Categories
                Article

                sin-quechers nano,d-spe,matrix effect,pesticide residue
                sin-quechers nano, d-spe, matrix effect, pesticide residue

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