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Simultaneous and Rapid Analysis of 500 Pesticide Multiresidues in Agricultural Products Using GC-MS/MS and LC-MS/MS : GC-MS/MS와 LC-MS/MS를 이용한 농식품 중 500개 잔류 농약 성분의 다성분 신속동시 분석 연구
DC Field | Value | Language |
---|---|---|
dc.contributor.advisor | 김정한 | - |
dc.contributor.author | 이종화 | - |
dc.date.accessioned | 2017-10-27T16:50:25Z | - |
dc.date.available | 2017-10-27T16:50:25Z | - |
dc.date.issued | 2017-08 | - |
dc.identifier.other | 000000145755 | - |
dc.identifier.uri | https://hdl.handle.net/10371/136900 | - |
dc.description | 학위논문 (박사)-- 서울대학교 대학원 농업생명과학대학 농생명공학부, 2017. 8. 김정한. | - |
dc.description.abstract | A multiresidue method for the simultaneous and rapid analysis of 500 pesticides in representative agricultural produce (brown rice, orange, spinach, and potato) was developed using a modified QuEChERS procedure combined with gas and liquid chromatography–tandem mass spectrometry (GC-MS/MS and LC-MS/MS). Multiple reaction monitoring parameters (e.g., collision energy, precursor and product ions) in MS/MS were optimized to achieve the best selectivity and sensitivity for a wide range of GC or LC-amenable pesticides. For the GC analysis of 360 pesticides, a short (20 m) microbore (0.18 mm i.d.) column resulted in better signal-to-noise (S/N) ratio with reduced analysis time than a conventional narrowbore column. The use of pulsed pressure injection was also effective to increase the peak response and S/N ratio. After changing a new liner, the priming injection, which caused by masking effect was suggested in order to consistent peak sensitivity. In LC-MS/MS analysis of 332 pesticides, the optimal mobile phase and injection volume was evaluated to acquire high sensitivity and reliable results. The limit of quantitation was <0.01 mg/kg, and the correlation coefficients (r2) of matrix-matched standards were >0.99 within the range of 0.0025–0.1 mg/kg. Acetonitrile with 0.1% formic acid without additional buffer salts was used for pesticide extraction, whereas only primary–secondary amine was used for dispersive solid phase extraction cleanup, to achieve good recoveries for most of the target analytes. The method was validated according to the European Union SANTE guidline.
The recoveries ranged from 70 to 120% with relative standard deviations of ≤20% at 0.01 and 0.05 mg/kg spiking levels (n = 6) in all samples, indicating acceptable accuracy and precision of the method. The results of matrix effects were indicated that mainly signal enhancements were observed in GC-MS/MS but in the LC-MS/MS, the evenly spread across the ranges and little difference within the samples. The optimized method was successfully applied to the analysis of pesticide residues in real samples. | - |
dc.description.tableofcontents | Introduction 1
Introduction to pesticide multiresidue analysis 1 Instrumental analysis in pesticide multiresidue 2 Principle of triple quadrupole-mass spectrometry 3 Gas chromatography-triple quadrupole mass spectrometry 10 Liquid chromatography-triple quadrupole mass spectrometry 14 Definition of terms relating to mass spectrometry 20 Trends in sample preparation method 25 QuEChERS methodology 35 Validation of analytical method 42 Matrix effect 49 The purpose of the present study 58 -Part 1 :Rapid and Simultaneous Analysis of 360 Pesticides in Crops Using Microbore GC-MS/MS 59 Materials and Methods 61 Chemicals and consumables 61 Analytical standard 61 Selection of GC column and instrumental conditions 62 Automated adjustment of retention time and retention indices 63 Pulsed pressure injection (PPI) parameters 64 Evaluation of peak sensitivity and column efficiency 64 Optimization of sample preparation 65 Final optimized sample preparation method 66 Priming effects 67 Validation of analytical methods 67 Matrix effects (ME) 68 Results and Discussion 70 Selected reaction monitoring (SRM) optimization 70 Retention time adjustment by AART 71 Selection of GC Column 75 Effect of pulsed pressure injection (PPI) 80 Comparison of column efficiency 80 Enhancement of peak sensitivity on a microbore column with pulsed pressure injection 83 Priming effects 88 Modification of Sample Extraction Solvent 94 Optimization of Sample Cleanup with dSPE 100 Method Validation 108 Matrix Effect (ME) 114 -Part 2: Rapid and Simultaneous Analysis of 332 Pesticides in Brown Rice, Orange, and Spinach Using LC-MS/MS 119 Materials and Methods 121 Chemicals and Consumables 121 LC-MS/MS instrumentation 121 Final sample preparation procedure 122 Validation of analytical method 123 Matrix effect 124 Results and Discussion 125 MRM optimization 125 Selection of mobile phase 126 Optimization of injection volume 127 Optimization of cleanup procedure 132 Method validation 135 Matrix effects 142 Real sample analysis 146 Conclusion 149 Supplementary Materials 150 References 201 Abstract in Korean 215 Literature Contributions 217 | - |
dc.format | application/pdf | - |
dc.format.extent | 2961224 bytes | - |
dc.format.medium | application/pdf | - |
dc.language.iso | en | - |
dc.publisher | 서울대학교 대학원 | - |
dc.subject | apple | - |
dc.subject | brown rice | - |
dc.subject | GC-MS/MS | - |
dc.subject | LC-MS/MS | - |
dc.subject | orange | - |
dc.subject | pesticide multiresidues | - |
dc.subject | potato | - |
dc.subject | QuEChERS | - |
dc.subject | spinach | - |
dc.subject.ddc | 630 | - |
dc.title | Simultaneous and Rapid Analysis of 500 Pesticide Multiresidues in Agricultural Products Using GC-MS/MS and LC-MS/MS | - |
dc.title.alternative | GC-MS/MS와 LC-MS/MS를 이용한 농식품 중 500개 잔류 농약 성분의 다성분 신속동시 분석 연구 | - |
dc.type | Thesis | - |
dc.description.degree | Doctor | - |
dc.contributor.affiliation | 농업생명과학대학 농생명공학부 | - |
dc.date.awarded | 2017-08 | - |
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