Agenda. Recent Advances in Detection of Heavy Metals in Foods. NQAC Organization

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Agenda Recent Advances in Detection of Heavy Metals in Foods NQAC Nestlé Quality Assurance Centre Supporting factors for reliable results? Daniel Hammer Nestlé Quality Assurance Centre Singapore 2...by never compromising on the safety and quality of our products so that our consumers can enjoy them with their eyes closed. NQAC Organization Global organization managed centrally by Corporate Quality Management (CO-QM) and was founded in 2010 consolidating the existing regional laboratories in one structure. The Nestlé Quality Assurance Center (NQAC) provides services to the Markets and Globally Managed Businesses (GMBs) in the area of food safety and quality management, and ensures that the company is prepared for new scientific developments or emerging food safety issues. NQAC Identity: 3 Dimensions Fast and reliable analytical services Food Safety/Quality Expertise Effectiveness of Food Safety and Quality Management 3 4

NQAC Global Organization 3 NQAC Zone Organisations (AMS, EMENA, AOA) > 25 NQACs Analytical Facilities > 40 Experts Delivering analytical services and technical assistance to markets and businesses 5 Analytical services provided by NQAC York Dublin Zhukowsky Rzeszow Weiding Padova Cergy Orbe Shoham Moga Dubai Vittel St. Louis Toluca Antigua Shah Alam Abidjan Sao Paulo Santiago Z-AMS (6) Z-EMENA (10) NQAC support factory labs in GLP (also auditing) and analytical competency building. NQACs approve 3rd party labs Tianjin NQACs target 7 calendar days TAT (5 working days ), in case of crisis NQAC need to have enough capacities and state of the art equipment to provide reliable data for decision making Navanakorn Cabuyao Singapore Clayville Nestlé approach for elemental analysis 7 Monitoring analysis on raw material and finished goods are carried out in NQACs. Release parameters are principally done by factory labs Nunspeet NQAC laboratories and their key methods are accredited Mulgrave Z-AOA (10) 6 Nestlé approach for elemental analysis History (the 2000s) AAS (GF/HG) ICP-OES ICP-MS ICP-MS (hyphenation and collision cells) 8

General Sample Preparation Quantitative determination of ten trace elements (Al, As, Cd, Co, Cr, Hg, Mo, Pb, Se and Sn) in all types of foodstuffs and raw materials including food grade salts by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) after pressure digestion. Mass spectrometers with additional reaction or collision cells are used to reduce the influence of polyatomic ions. The method has been validated in-house for all foodstuffs covering AOAC food triangle. The method is based on official CEN standard EN 13805:2013 for high pressure digestion, standard EN 15763:2009 for As, Cd, Hg and Pb, EN 15765:2009 for Sn and AOAC 2011.19 for Cr, Mo and Se with modifications on the sample preparation and analytical conditions. Weighing of 0.25g sample into Quartz tubes, adding of HNO3 ultrapure, capping and sealing with Teflon tape Around 45 minutes run in HPA. Complete digestion under nitrogen pressure. Filtering may not be necessary 9 10 Sample preparation and importance of decontamination Sample preparation for heavy metal analysis in foods importance of decontamination To avoid such spread of results due to contamination, extreme care must be taken. Clean environment: closed lab, covered autosampler. Sample handling in fumehoods Clean material: Ultrapure acid (subboiled), quartz tubes or teflon tubes decontaminated, if filters are used, check their quality, reagent blank check! Covered autosampler Closed lab 11 12

preparation and importance of decontamination Sample under fumehoods Subboiled acid 13 Sample - additional features for reliable results Matrix effects to compensate for (e.g. Carbon effect) Ultrapure Water For constant signal add IPA at 2% continuously Matrix effect leading to fluctuation of signal (use internal standard added continuously) Decontamination of digest tubes - additional features for reliable results 14 NQACs and Accreditation Polyatomic interferences suppression with collision or reaction gas (He, NH3) 15 16 Success factor for reliable results

Analytical methods development continuous activity in Nestlé R&D Some principles Analytical method should be based on existing international standards Where no such standards exist development is conducted by R&D and method published internally as Laboratory Instructions. Methods should be published if applicable in order to make it accessible to others R&D is to be involved in international standards creation/maintenance: participation in international working groups (AOAC, Codex, CEN, ISO, IDF etc.). Analytical methods development Nestlé being part of standards committees Nestlé developing standards 17 18 Analytical methods deployment: Integrated workflows between sites (NRC vs NQACs) On board early in development phase Connected regularly with NRC via Telco Smooth implementation, in parallel of method validation Global projects between NRC and multiple NQACs (e.g. Quechers) NRC: global coordination, setting up key pesticide lists, method development in partnership with ZNQACs NQACs: validation of method under NQAC conditions Maggi in India NQAC SG provided 400 results within 8 days. NQAC SG assisted 6 other markets with analyses Results compared very well with other NQACs and Nestle approved 3 rd party labs. results comparison 20

Summary What makes an analytical method successful: Research & Development that takes into account customer needs (fit for purpose vs matrices, speed, reliability) Published in peer reviewed journal Aligned with international standards for comparability Embedded in the context of quality assurance and management (adapted lab environment, interlab tests, available reference material, ACCREDITATION) For 15 years ICP-MS approach established within over 10 NQACs 21