Summary of analytical Chemistry doctoral thesis: Study and development of QuEChERS GC/MS 3 SIM technique to analyze multi pesticide residues in soil
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Develop a rapid and simple method for analysis of multi-residue pesticides, including organophosphate, organochlorine, carbamate, and pyrethroid compounds in soil, with sample preparation based on QuEChERS technique and determination by GC-MS.
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Summary of analytical Chemistry doctoral thesis: Study and development of QuEChERS GC/MS 3 SIM technique to analyze multi pesticide residues in soilMINISTRY OF EDUCATION AND VIETNAM ACADEMY TRAINING OF SCIENCE AND TECHNOLOGY GRADUATE UNIVERSITY SCIENCE AND TECHNOLOGY ----------------------------- Pham Tuan LinhSTUDY AND DEVELOPMENT OF QuEChERS GC/MS 3 SIMTECHNIQUE TO ANALYSE MULTI PESTICIDE RESIDUES IN SOIL Major: Analytical Chemistry Code: 62.44.01.18 SUMMARY OF ANALYTICAL CHEMISTRY DOCTORAL THESIS Hanoi, 2019 2 This thesis is completed at: Graduate University Science and Technology – Vietnam Academy of Science and Technology.Science instructor 1: Assoc.Prof.Dr. Vu Duc LoiScience instructor 2: Assoc.Prof.Dr. Nguyen Hong KhanhReviewer 1:Reviewer 2:Reviewer 3: The thesis will be presented to the scientific councilat Graduate University Science and Technology – Vietnam Academy of Science and Technology at …..… h .., date …… month …….. , 2019The thesis can be found at:- Library of Graduate University Science and Technology- National library of Vietnam 3 INTRODUCTION 1. The urgency of the thesis Nowadays, more than1500 different kinds of pesticides havebeen used, classified based on chemical structure (chlorinated,phosphorus, Carbamate, Pyrethroid ...) or by application (insecticide,fungicide, herbicide ...) In Vietnam, more and more different pesticides are used inagriculture (increased from 189 substances in 2003 to 437 substancesin 2010). Pesticides have been known to be contaminants that persistfor a long time in the environment. So over time, there will beresidues of many different pesticide in the soil. Pesticides accumulated in the soil can be transferred tohumans via the food chain, being potentially harmful to humanhealth. Thus, the level of pesticide residues in the agricultural soilneeds to be monitored as farmers switch to organic farming (greenand safe agriculture) Currently, pesticide residues in soil is determined separatelyfor each substance group, with different procedures, so increasingcosts, extend the analysis time and analysis process becomes morecomplicated. Therefore, the project Study and development ofQuEChERS GC / MS 3 SIM technique to analyze multi pesticideresidues in soil was carried out, in order to reduce the analysis time,minimize the number of analytical steps, use fewer reagents insmaller amounts and provide high recovery 4 2. Scope of thesis Develop a rapid and simple method for analysis of multi-residuepesticides, including organophosphate, organochlorine, carbamate,and pyrethroid compounds in soil, with sample preparation based onQuEChERS technique and determination by GC-MS. 3. Main contents of thesis- Survey and select optimal conditions to analyze multi pesticides onGC / MS system: injection mode, temperature program, parametersfor mass spectrometry.- Investigate optimization of processing samples includingextraction, cleaning and enrichment: solvent and extraction time,influencing factors, cleaning agents.- Verification of analytical methods: determination of linear range,calibration curve, detection limit and quantitative limit, recoverycoefficient and repeatability of the method.- Apply the optimal procedure to analyze 30 soil samples andcompare results with 04 laboratories at Vietnam and Korea 4. New contributions of the thesis- This is the first study in Vietnam to apply the QuEChERS method for multi-residues pesticides analysis in the soil- d-SPE has been applied instead of soxhlet extraction, so the sample preparation time has been reduced from 24 h to 25 minutes, consuming only 15 ml solvent (the popular methods consume at least 300ml of solvent)- With a single run, 103 pesticides in soil have been analyzed (the latest publication, only 42 pesticides in the soil were quantified)- In quantitative step, only GC/MS is used (in publications, GC/MS/MS is analytical method usually selected) 5 CHAPTER 1. OVERVIEW Pesticides (herbicides, fungicides or insecticides) areenvironmental pollutants often found in soil, water, atmosphere andagricultural products, and may exist in harmful levels, posing anenvironmental threat. Even low levels of pesticide can cause adverseeffects on humans, plants, animals and ecosystems. The applicationof pesticides has increased appreciably during the past few decades,resulting in a potential ...
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Summary of analytical Chemistry doctoral thesis: Study and development of QuEChERS GC/MS 3 SIM technique to analyze multi pesticide residues in soilMINISTRY OF EDUCATION AND VIETNAM ACADEMY TRAINING OF SCIENCE AND TECHNOLOGY GRADUATE UNIVERSITY SCIENCE AND TECHNOLOGY ----------------------------- Pham Tuan LinhSTUDY AND DEVELOPMENT OF QuEChERS GC/MS 3 SIMTECHNIQUE TO ANALYSE MULTI PESTICIDE RESIDUES IN SOIL Major: Analytical Chemistry Code: 62.44.01.18 SUMMARY OF ANALYTICAL CHEMISTRY DOCTORAL THESIS Hanoi, 2019 2 This thesis is completed at: Graduate University Science and Technology – Vietnam Academy of Science and Technology.Science instructor 1: Assoc.Prof.Dr. Vu Duc LoiScience instructor 2: Assoc.Prof.Dr. Nguyen Hong KhanhReviewer 1:Reviewer 2:Reviewer 3: The thesis will be presented to the scientific councilat Graduate University Science and Technology – Vietnam Academy of Science and Technology at …..… h .., date …… month …….. , 2019The thesis can be found at:- Library of Graduate University Science and Technology- National library of Vietnam 3 INTRODUCTION 1. The urgency of the thesis Nowadays, more than1500 different kinds of pesticides havebeen used, classified based on chemical structure (chlorinated,phosphorus, Carbamate, Pyrethroid ...) or by application (insecticide,fungicide, herbicide ...) In Vietnam, more and more different pesticides are used inagriculture (increased from 189 substances in 2003 to 437 substancesin 2010). Pesticides have been known to be contaminants that persistfor a long time in the environment. So over time, there will beresidues of many different pesticide in the soil. Pesticides accumulated in the soil can be transferred tohumans via the food chain, being potentially harmful to humanhealth. Thus, the level of pesticide residues in the agricultural soilneeds to be monitored as farmers switch to organic farming (greenand safe agriculture) Currently, pesticide residues in soil is determined separatelyfor each substance group, with different procedures, so increasingcosts, extend the analysis time and analysis process becomes morecomplicated. Therefore, the project Study and development ofQuEChERS GC / MS 3 SIM technique to analyze multi pesticideresidues in soil was carried out, in order to reduce the analysis time,minimize the number of analytical steps, use fewer reagents insmaller amounts and provide high recovery 4 2. Scope of thesis Develop a rapid and simple method for analysis of multi-residuepesticides, including organophosphate, organochlorine, carbamate,and pyrethroid compounds in soil, with sample preparation based onQuEChERS technique and determination by GC-MS. 3. Main contents of thesis- Survey and select optimal conditions to analyze multi pesticides onGC / MS system: injection mode, temperature program, parametersfor mass spectrometry.- Investigate optimization of processing samples includingextraction, cleaning and enrichment: solvent and extraction time,influencing factors, cleaning agents.- Verification of analytical methods: determination of linear range,calibration curve, detection limit and quantitative limit, recoverycoefficient and repeatability of the method.- Apply the optimal procedure to analyze 30 soil samples andcompare results with 04 laboratories at Vietnam and Korea 4. New contributions of the thesis- This is the first study in Vietnam to apply the QuEChERS method for multi-residues pesticides analysis in the soil- d-SPE has been applied instead of soxhlet extraction, so the sample preparation time has been reduced from 24 h to 25 minutes, consuming only 15 ml solvent (the popular methods consume at least 300ml of solvent)- With a single run, 103 pesticides in soil have been analyzed (the latest publication, only 42 pesticides in the soil were quantified)- In quantitative step, only GC/MS is used (in publications, GC/MS/MS is analytical method usually selected) 5 CHAPTER 1. OVERVIEW Pesticides (herbicides, fungicides or insecticides) areenvironmental pollutants often found in soil, water, atmosphere andagricultural products, and may exist in harmful levels, posing anenvironmental threat. Even low levels of pesticide can cause adverseeffects on humans, plants, animals and ecosystems. The applicationof pesticides has increased appreciably during the past few decades,resulting in a potential ...
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