NATIONAL FOOD ADMINISTRATION Multi-residue Methods used for Pesticides Residues Analysis of Fruits and Vegetables in Sweden Arne Andersson National Food Administration Sweden

NATIONAL FOOD ADMINISTRATION Analytical method A multi-residue method (M001/101) using ethyl acetate extraction and GPC clean-up was the main method during Determination of residues was done using GC (ITD, ECD, FPD, NPD) and HPLC Scope: about 200 pesticides and metabolites in one single analysis For acidic crops, NaOH was added and a new extraction was carried out (M002/102)

NATIONAL FOOD ADMINISTRATION Determination by LC-MS/MS and GC equipped with conventional detectors In 2004 the HPLC determination was replaced by LC-MS/MS No GPC clean-up was needed Sensitive and selective provides quantification and confirmation at the same time LOQ: 10 ppb (0.01 mg/kg) for most pesticides

NATIONAL FOOD ADMINISTRATION The new extraction procedure for all crops, used from 1 January 2005 Ethyl acetate and addition of 15 g NaHCO 3, to all crops. This increased the pH to 6-8 in acidic fruits and vegetables By this small change two old multi-methods could be substituted by one new method (M200) The determination is carried out by LC-MS/MS, GC-ITD and GC-ECD

NATIONAL FOOD ADMINISTRATION

NATIONAL FOOD ADMINISTRATION

NATIONAL FOOD ADMINISTRATION Benefits of using LC-MS/MS determination No GPC clean-up is needed Selective, provides quantification and confirmation at the same time Better reproducibility for polar pesticides compared with GC LOQ: 10 ppb (0.01 mg/kg) for most pesticides

NATIONAL FOOD ADMINISTRATION Change to GC-MS/MS determination The goal is to change from using GC –ITD and GC-ECD to GC-MS/MS by 1 July 2006

NATIONAL FOOD ADMINISTRATION

NATIONAL FOOD ADMINISTRATION

NATIONAL FOOD ADMINISTRATION

NATIONAL FOOD ADMINISTRATION EU Analytical Quality Control Guidelines The revised version: SANCO/10232/2006, 24 March 2006 “Quality Control Procedures for Pesticide Residues Analysis” Major updates: Confirmation using LC-MS/MS and GC-MS/MS Uncertainty and enforcement Organizer: Tuija Pihlström, National Food Administration, Sweden

NATIONAL FOOD ADMINISTRATION EU Proficiency Test 7, 2005 List with 62 pesticides 16 of the pesticides were applied to a sample of grapes 125 labs in 27 countries participated Satisfactory results (Z-scores <2): 79 – 96% for the individual pesticides present Organizer: Amadeo Fernández-Alba, University of Almeria, Spain

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