| Traditional detection methods of pesticiedes or other pollutants were mostly based on large-scale testing equipment,and the process of sample preparation was complicated,which could be unable to realize the rapid detection on site.Ion mobility spectrometry(IMS)is an new kind of investigation and seperation technique which has advantages of quickness,sensitiveness,convenience and low cost,and it has played a very particular role in field testing of explosives and neurotoxic.In this study,analytical methods based on pulse glow discharge-ion mobility spectrometry(PGD-IMS)and sample rapid pretreatment were developed for rapid analysis of representative pesticide and other harmful pollutant residues in environment and agricultural products.More than 100 kinds of harmful pollutants were tested by positive PGD-IMS,and K0 of nearly 100 kinds of components were calibrated,including pesticide,veterinary drug,and other harmful pollutant,and PGD-IMS standard material library was established.An analytical method based on multiwalled carbon nanotubes(MWCNTs)dispersive solid-phase extraction coupled with PGD-IMS was developed for analysis of 30 pesticide residues in water samples.Reduced ion mobilities and mass-mobility correlation of 30 pesticides were measured.The extraction conditions were optimized.The detection limits of pesticides were 0.01～0.77 μg kg-1.The method was applied for the analysis of practical and spiked water samples.All results were confirmed by HPLC-MS/MS.An analytical method based on stir bar sorptive extraction(SBSE)coupled with PGD-IMS was developed for analysis of three triazine pesticide residues in water and soil samples.An injection port with sealing device and stir bars hold device were applied,making desorption and detection of analytes proceeded simultaneously.Three kinds of stir bar coating were made,and the extraction conditions were optimized.The LODs and LOQs of three triazines were found to be 0.006-0.015μg kg-1 and 0.02-0.05 μg kg-1.The proposed method was environmentally friendly without organic solvent consumption in the entire experimental procedures.And the proposed method was applied for the analysis of real ground water,surface water and soil samples.The research explore the mobility and distribution rules of simazine,acetamiprid,hexazinone,paclobutrazol,amitraz,clofentezine and boscalid in pulp and peel of apple,cucumber and cherry tomato,and rapid analysis of pesticide residues on fruits and vegetables surface by IMS.A lab test was carried out by treating the matrices with standard solution.The percentage sorption of pesticides and the ratio values(Q)between pulp and peel concentrations in three matrices were were measured.In addition,a rapid and simple process combining surface swab capture method and PGD-IMS detection was established for detection of pesticides on matrix surfaces.The releasing factors(RF)of pesticides in three matrices were calculated.The linearity,LOD,LOQ and matrix effect were investigated to assess the proposed method.The LOD and LOQ of 7 pesticides were 1-3 and 3-10 μg kg-1,respectively,and the method was applied for the analysis of real samples.The mobility and distribution rules of 24 pesticides in pulp and peel of apple,cucumber and eggplant were investigated.A lab test also was carried out by treating the matrices with standard solution.The Qs were measured in three matrices.A field test using commercial formulations containing 5-9 pesticides for each matrix,and the Qs were measured in field.In addition,surface swab capture method and PGD-IMS detection was established for detection of pesticides on matrix surfaces.The kind of elution solvent was optimized,and the RFs of pesticides in three matrices were calculated.The linearity,LOD and LOQ matrix effect were investigated to verify the swab-IMS process.The RFs of pesticides eluted by acetonitrile were in the range of 30.4-107.3%,and LOD and LOQ of 24 pesticides were 0.3-3 and 1-10 μg/kg,respectively.The swab-IMS method is rapid,sensitive,and can be achieved in the field.Analytical method based on multiplug filtration cleanup(m-PFC)method coupled with PGD-IMS was developed for analysis of MS-222 residue in fish and fish-raising water samples.The extraction solvent and purification process were optimized.At the same time,IMS and LC-MS/MS methods were established.IMS system could be used a rapid screening tool on site with the advantage of rapid,simple and portable,and HPLC-MS/MS system could be used for results validation in laboratory conditions with the advantage of lower limit of detection,and was more stable and precise.IMS was proven to be a commendable rapid screening qualitative and semi-quantitative technique for analysis of pesticide and other pollutant residues in environment samples and agricultural products on site. |
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