Pesticide residue analysis: New Trends. Michal Godula, Ph.D. EU Marketing Manager Food Safety & Environmental Thermo Fisher Scientific

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1 Pesticide residue analysis: New Trends Michal Godula, Ph.D. EU Marketing Manager Food Safety & Environmental Thermo Fisher Scientific

2 Why pesticide analysis? Extensively used in agriculture to control pests & improve yields More than 1000 different active substances used Thoroughly tested and evaluated before approval BUT Sometimes not applied in accordance with intended purpose GAP sometimes not respected Signicant public concerns about pesticide use Regulatory requirements 1 1

3 Pesticide facts 2001 WW Pesticide usage 2006, UK mygraphresults.cfm 2 2

4 EU Pesticide residue regulations Until 1 September 2008 legislation only partially harmonized EU- MRLs ± 250 pesticides National MRLs ± 850 pesticides 76/895/EEC (fruits and vegetables) 86/362/EEC (cereals) 86/363/EEC (animal products) 90/642/EEC (fruits and vegetables) No harmonized risk assessment for EU consumers, Trade problems Regulation 396/2005 > 490 pesticides > MRLs General MRL 0.01 mg/kg 3 3

5 EU pesticide monitoring programs Number of pesticides analyzed: up to 700 Baby food samples > MRL: 0.2% 2008 Annual Report on Pesticide Residues EFSA Journal 2010; 8(6):

6 Workflow for analysis of pesticide residues 5 5

7 Challenges of pesticide residue analysis Sample variability (matrix) Different compound characteristics Number of samples Number of analytes monitored Low levels controlled ( <10 ng/g ) Fast response required 6 6

8 Sample preparation: Key step to success Cryogenic milling effect on pesticide levels Fussell, et al. (2007) Food Additives & Contam., 24:

9 Analytical method parameters to optimize: Performance Costs Speed 8 8

10 Sample preparation by QuEChERS For: moisture > 75%, low fat fruits and vegetables LOQ: < 10 ng/g 229 pesticides AOAC Method Sample Extraction Centrifugation Dispersive SPE Centrifugation Determination 9 9

11 Simplified sample preparation challenges Clean-up efficiency Detection selectivity Simple extraction QuEChERS LLE GPC SPE IAC Orbitrap MS MS/MS LC-MS GC-MS HPLC-FLD HPLC-UV GC-ECD, NPD 10 10

12 Routine lab requirements Simplified sample preparation Fast analysis (screening and confirmation in one run) Rapid data evaluation LOW COSTS! While LOQs/RSDs achieved Confidence in results Easy to use Low maintenance and running costs 11 11

13 Mass spectrometry in pesticide analysis Simple sample preparation: QuEChERS, extract-n-shoot Targeted analysis and quantitation using Single and Triple Quadrupoles (SIM, SRM) coupled to LC (UHPLC) and GC Sample QuEChERS GC/MS/MS LC/MS/MS Limited screening capability of MS/MS (~ compounds) Data evaluation is time consuming Multiple instruments to cover whole scope of method Limited information contained 12 12

14 Alternative approach: Non targeted data acquisition Non-targeted analysis using Full Scan MS instruments Time-of-Flight or Orbitrap instruments: excellent mass accuracy and resolution Sample All data acquisition Data evaluation Accurate mass search Spectral library search Quantitation/ Confirmation Reporting 13 13

15 Benefits of High Resolution approach Non targeted acquisition (all info gathered) No analyte specific setup: 1 set of conditions Theoretically unlimited number of analytes Meeting analytical criteria (LODs, RSDs) Multi-methods possible (pesticides+mycotoxins) Retrospective data analysis (unknowns) 14 14

16 But: data acquired is enormous Data extraction from raw files Simplification of data Screening against libraries Confirmation/Quantification Reporting (instrument reports) Laboratory Information management System (LIMS) Customer Report 15 15

17 Pesticide residues - outlook Multi-residue methods are a must - save time and costs In routine pesticide analysis costs/throughput and performance will be the requirements New technology (High Resolution MS) provides tools to extend scope of methods Data managements streamlining will help to reduce costs Direct sample analysis is to be explored (DART-MS) 16 16

18 Food Safety is a Global Issue 17 17

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