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The Study on the Sample Pretreatment for Sulfonylurea Herbicides and Benzoylureas Pesticides Residues Analysis

Author: LiuJinXia
Tutor: HuangZhiQiang；ChenBo
School: Hunan Normal University
Course: Analytical Chemistry
Keywords: Pesticide residues Food of animal origin Solid Phase Extraction High performance liquid chromatography - tandem mass spectrometry Fe3O4 submicron ball
CLC: TS207.53
Type: Master's thesis
Year: 2011
Downloads: 96
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Abstract


Pesticide residues in food has always been highly concerned about food safety issues in the international community. U.S., EU and Japan and other developed countries more and more strict control of pesticide residues, maximum residue limits of pesticides as low as ppb level. Therefore, the establishment of high selectivity, high sensitivity detection of pesticide residues method has been the core of government oversight bodies, as well as the research department. With the rapid development of the terminal detection equipment, sample pre-treatment and gradually became the bottleneck step in the analysis of pesticide residues in the entire process. Therefore, the sample pre-treatment in the analysis of pesticide residues is particularly important. This thesis focuses on the of sulfonylurea and Benzoylurea pesticide residue analysis in sample pretreatment methods and a series of studies, and the establishment of a rapid enrichment of Fe3O4 submicron ball extraction, separation and purification ago Processing method. Combined with high performance liquid chromatography - tandem mass spectrometry detection technology, higher sensitivity, better selectivity sulfonylurea and benzoyl urea pesticide residue analysis method. Thesis work is as follows: 1. Food of animal origin 20 sulfonylurea herbicides multi-residue analytical methods. Using Waters Oasis HLB solid phase extraction column enrichment of sulfonylurea herbicides residues in the samples was measured by HPLC-MS2, 20 sulfonylurea 2.5μg / L ~ 200μg / L range, the linear correlation coefficient greater than 0.998, the minimum detection limit of 0.5 pg / kg; method recoveries ranged between 66.07% -112.07%. Method of anti-interference ability, simple operation, high sensitivity, good universality, the analysis can be applied to different types of food of animal origin. (2) the establishment of a multi-residue pesticide analysis methods the 10 kinds Benzoylurea pork. Compare inspection gel permeation chromatography (GPC) and neutral alumina (Alumina N) solid phase extraction pork benzoyl urea determination of pesticide residues in purifying effect, the results show that the two methods can achieve the removal of pork The purpose of the high content of fat and protein matrix. 10 Benzoylurea drugs 1μg / L ~ 100μg / L within the linear correlation coefficient greater than 0.9982 minimum detection limit 0.125μg / L, Alumina N solid-phase extraction (SPE) purification method recovery was 65.6% to 101.7%, the GPC purification method recovery was 76.5% to 96.6%. The results confirmed that the two purification methods can be used for pork samples of effective purification, for pork Benzoylurea pesticides, residue analysis of the sample pre-treatment provides more options. 3. Fe3O4 submicron ball extraction of trace benzoyl urea insecticides pre-treatment method. Solvothermal reduction synthesis Fe3O4 submicron ball, to get the magnetic Fe3O4 sub-micron particle size uniformity ball, and investigate the feasibility of enrichment of trace amounts of benzoyl urea insecticides extraction. By optimizing the various extraction conditions (pH, adsorption saturation, contact time and elution solvent), successfully applied to the water for 5 Benzoylurea pesticide residue analysis. 5 Benzoylurea drugs in the range of 1μg / L ~ 100μg / L, the linear correlation coefficient greater than 0.9990 minimum detection limit 0.125μg / L, the actual water samples spiked recoveries ranged from 67.5% to 89.7%. Compared with the GPC and SPE, the newly created method has the advantages of simple equipment, time is short, the organic solvent consumption, green.

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CLC: > Industrial Technology > Light industry,handicrafts > Food Industry > General issues > Food standards and testing > Determination of food contamination > Determination of pesticide residues
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