Applications of advanced instrumental analytical techniques in the field of pesticide formulations
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1 Applications of advanced instrumental analytical techniques in the field of pesticide formulations Impurities, illegal, counterfeit, spraying solutions and unknown samples George P. Balayiannis Laboratory of Chemical Control of Pesticides
2 Instrumental Analytical Techniques For formulations HPLC-UV GC-FID Determination of active ingredients Impurities
3 HPLC-UV: cymoxanil cymoxanil acetophenone
4 GC-FID: alpha-cypermethrin Applications of advanced instrumental analytical techniques
5 GC-FID: chlorothalonil Applications of advanced instrumental analytical techniques
6 Advanced Instrumental Analytical Techniques Instrument Configurations LC-MS LC-MS/MS GC-MS GC-MS/MS Extreme cases High resolution MS NMR X-ray electronic microscope Ionization techniques Electrospray Ionisation Atmospheric Pressure Ionization (ESI- APCI) Electron Ionization- Negative/Positive Chemical Ionization (EI-NCI- PCI)
7 Advanced Instrumental Analytical Techniques Analysis of Samples with strong interference to the target analyte Small concentrations of target analytes Screening-Non target analysis Chromatographic profiling Target analytes impurities relevant impurities (hexachlorobenzenenitrosamines) active ingredients (wrong active ingredients, unknown samples, spraying solutions, a.i. that do not resolve chromatographically) Co-formulants
8 Samples with strong interference to the target analyte Carbendazim in sulphur formulations (organic farming) HPLC-UV analysis
9 Samples with strong interference to the target analyte Carbendazim in sulphur formulations (organic farming) LC-MS/MS analysis (192>160) formulation white particles Standard solution carbendazim 0.05 μg/ml
10 Small concentrations of target analytes active ingredients Non-registered/wrong-irrelevant active ingredients Relevant impurities Confirmation and/or quantification
11 Low-quality PPP Applications of advanced instrumental analytical techniques Small concentration of targeted analytes Wrong active ingredient present in the formulation Herbicide in insecticide: prometryne found in trace amounts in insecticide formulation (GC-MS/MS) Relevant impurity: hexachlorobenzene in chlorothalonil (limit 0.04 g/kg) Application of FAO GC-MS method
12 Screening-Non target analysis Identification of compounds in spraying solutions that caused damage samples with small amounts of a second active ingredient Unknown-unlabeled samples GC-MS (libraries) LC-MS (molecular ion)
13 Spraying solutions Caused damage Traces of foramsulfuron were detected with LC-MS and confirmed with LC-MS/MS Applications of advanced instrumental analytical techniques Non target analysis Illegal-unknown formulations Unregistered thiodicarb formulation with no label Detected with LC-MS and confirmed with LC-MS/MS
14 Low-quality PPP Sample with small amounts of a second active ingredient Applications of advanced instrumental analytical techniques Non target analysis Herbicide in fungicide: oxyfluorfen found in sample of fungicide formulation (GC-MS/MS) GC-MS full scan oxyfluorfen GC-MS/MS
15 Co-formulants and solvents Chromatographic profile GC-MS LC-MS
16 Chromatographic Profiling Co-formulants and solvents Chromatographic profile comparison
17 Determination with LC-MS/MS of PPP active ingredients that do not resolve chromatographically ΜCPA 2,4 D Sample
18 PPP Market Conclusion Demanding Legal Framework Increasing number of out of the ordinary samples Laboratory Modern analytical equipment Application of advanced analytical techniques
19 THANK YOU FOR YOUR ATTENTION! ANY QUESTIONS?
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