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WORKING MATERIAL
Coordinated Research Project (CRP): D5.20.38
Accessible Technologies for the
Verification of Origin of Dairy Products
as an Example Control System to
Enhance Global Trade and Food Safety
REPORT OF THE 1ST
RESEARCH COORDINATION
MEETING.
Vienna, Austria, November 26-29, 2013.
NOTE
The material in this document has been agreed by the participants and has not been edited by the
IAEA. The views expressed remain the responsibility of the participants and do not necessarily
reflect those of the government(s) of the designating Member State(s). In particular, neither the IAEA
nor any other organization or body sponsoring this meeting can be held responsible for any material
reproduced in the document.
Reproduced by the IAEA
Vienna, Austria, 2013
INTERNATIONAL ATOMIC ENERGY AGENCY
Report of the 1st
Research Coordination
Meeting (RCM) on Accessible
Technologies for the Verification of
Origin of Dairy Products as an Example
Control System to Enhance Global Trade
and Food Safety
Vienna, Austria, 26-29 November 2013
Working Material Produced by the IAEA
Vienna, Austria, 2013
2
Introduction
The 1st Research Coordination Meeting (RCM) for the Coordinated Research Project (CRP)
on “Accessible Technologies for the Verification of Origin of Dairy Products as an Example
Control System to Enhance Global Trade and Food Safety” was held at the Vienna
International Centre, Vienna, November 26 – 29 2013.
The Meeting was chaired by the Scientific Secretary, Russell Frew (IAEA). Ms Preeni
Abeynayake (Sri Lanka, Contract No. 18066) was Rapporteur. A list of participants and the
meeting Agenda are annexed to this report.
The RCM was formally opened by Mr Andrew Cannavan, Head, Food and Environmental
Protection Laboratory, IAEA, who in his opening speech highlighted the importance of this
CRP in the programme of the Food and Environmental Protection Section of the IAEA.
Traceability systems are a key component of food safety not only providing consumer
protection but also enhancing trade. Nuclear techniques play an important role in the
verification of origin and hence the IAEA is very supportive of these activities. It is expected
that the systems and procedures developed through this CRP will benefit Member States to
obtain better market access and higher process for their commodities in the global market.
Objectives of the Research Coordination Meeting
The meeting commenced with a presentation from the Scientific Secretary on the current
activities of the Food and Environment Protection Section and the objectives of the CRP and
the RCM. The meeting was reminded that the main aims of this RCM was to:
1) Evaluate and discuss the aim and objectives of the project;
2) Prepare work plans for the next phase of the project (2014);
3) Facilitate a broader understanding of the relationship each participant has to the
overall objectives of the CRP and to promote interaction between the participants;
4) Prepare recommendations and guidelines to facilitate project tasks and for the
participants to agree a common approach and way forward;
5) Identify specific needs of participants that the IAEA could actively support. These
may include training, provision of advice and analytical support.
The Meeting was also reminded that the main objective of the CRP was to develop an end-to-
end system for verification of the origin of food products. Dairy products were chosen as the
commodity to work on for this project for many reasons including their global production,
high level of trade, consumer sensitivity to fraud and scope for applying a wide range of
analytical techniques. It is intended that the system developed for tracing origin of dairy
products will be used as a template that can be applied to other commodities. Therefore the
participants were encouraged to think of the entire system including environment, production
practices, analytical approaches, mapping and interpretation and consumer access to the
technology. An expected outcome of the programme is a network of laboratories of FAO and
IAEA member states. In this regard the importance of preparing Standard Operating
Procedures (SOPs) with appropriate validation data was stressed.
3 3
RCM Presentations.
The Research Contract Holders each made presentations of their planned work. These
presentations scoped out the type of dairy production in each country. It was evident that
there is a wide range of dairy systems represented in the project; from small individual
producers through to giant collectives. This is very good for the future extrapolation of the
results from this research to other member states. However, it does present challenges in
terms of the project logistics and ensuring a coherent approach across all individual projects.
Following the presentations the key issues for the overall project were identified and the
meeting participants divided into two working groups to discuss them. The issues identified
and discussed included;
1) Data quality and the need for standard operating procedures;
2) Sampling, particularly whether a set of core samples should be collected by each
contract holder and be made available to the project as a whole;
3) What core analyses should be performed to build a coherent dataset?
4) What metadata should be collated?
To some extent the analytical approach is governed by the analytical capability of the
participants. The available instrumentation and expertise/ experience available to each
participant were identified and a summary is presented in Annex III, which shows that the
project is well supported in terms of analytical capability.
Since the individual projects are being conducted in very different settings, discussion was
held on how to facilitate their integration into a coherent body of work. It was decided that
background information and particulars from each project be collated and stored on the
project website. The list of background data requested is given in Annex IV. In addition a
table of parameters to be compiled as metadata with each sample was decided upon (also
Annex IV).
One of the working groups discussed aspects of the sampling strategy and logistics. The full
report from that group can be found in Annex V. Briefly, the key points raised were:
o The initial sampling strategy will aim to provide information to characterize the
chemical variability within and between regions, and relationships with environmental
drivers. To assist the decision-making for sampling Principle Investigators should
compile as much information as possible on characteristics and practices (what
products, production quantities, catchment area, rearing practices, watering regimes,
feeding practices).
o The group will use common spreadsheets with information for each region. This
information will be shared and used to create maps.
o Samples should be collected 3 times per year from any given producer.
o Monthly precipitation sampling is encouraged to compliment the precipitation isotope
maps available through activities such as GNIP and WaterIsotopes.org, etc. A protocol
based on experience gained in the New Zealand precipitation mapping project will be
made available.
o Each group is encouraged to try to develop relationships with producers to collect some
samples that they can verify the authentic origin of.
4 4
Activity: comparing authentic (origin-verified) with commercial samples from the
same producer. Where commercial samples are to be collected, effort should be
made to collect authentic samples at the same time for subsequent comparison.
Sampling protocols for milk, rainfall, and soils are required.
Once the global project parameters were set the Research Contract Holders worked with the
Agreement Holders and the Observers to revise and finalise their individual work plans and
formulate their planned activities and milestones for the next phase of the project. The
individual contract work plans are appended in Annex VI.
Conclusions:
The meeting recognized that this CRP has initiated collaboration between laboratories
(network of laboratories) of different member states and that it provides information
that can have a regulatory impact, e.g. the detection of milk whose chemical parameters
do not comply with that from the claimed origin may be an indication of fraud.
Each Research Contract Holder’s work was reviewed to ensure that high scientific
standards and the objectives of the CRP were met and their work plans, activities and
deliverables for the next phase of the project were finalised. The discussions led to a
high level of coherence between participants and this is reflected in the finalised work
plans.
To ensure that a primary objective of the CRP to populate a database with high-quality
data from authentic-origin is met, it was agreed that the core methods developed and
used by the contract holders will be presented as SOP’s with appropriate validation
data. Agreement Holders will provide assistance where needed.
The focus of the first phase of the project is to ensure harmony of methods and data
quality between participants. Sampling in the first stage will focus on obtaining
samples of authentic origin to enable maps of the spatial variability in parameters to be
made. Later in the project the focus may turn to imported/ traded milk products but the
interpretation of that data relies on having the spatial maps in place.
An objective of the overall programme is to develop tools for rapid response based
around recent developments in laser-based analytical technologies. However only one
contract holder has access to a laser system for stable isotope analysis. Support will be
sought from manufactures to assist with the development of fit-for-purpose methods
based on this instrument. Prof. Almirall (agreement holder, FIU) will proceed with a
project utilising Laser Induced Breakdown Spectroscopy. It was recognised that a
support through a technical contract may be required.
It was recognised that the time required to obtain appropriate import licences for
reagents and biological samples should not be underestimated. Failure to comply with
import regulations could mean the refusal of a carrier to transport the material or cause
delays in customs clearance. It was agreed that Contract Holders will examine their
national regulations concerning export/import of biological and chemical materials and
standards and put in place all the necessary clearances before shipment.
5 5
Recommendations.
1) A core set of samples should be collected by each agreement holder. These samples
will be a resource to the overall project.
2) Protocols for sampling, sample preparation and analysis should be provided to the
group. Recommended procedures for light stable isotope analysis of dairy should be
compiled into a technical document or small book. Other protocols should be obtained
from previous studies e.g. EU Trace, NZ CDRP.
3) The following reference materials should be purchased by each contract holder:
a. IAEA-600 Caffeine (C, N) Solid
b. IAEA-601 Benzoic Acid (O) Solid
c. IAEA-CH-7 Polyethylene (C, H) Solid
d. NBS22 (C,H) Oil, may be substituted for IAEA-CH-7
4) Water of known H and O isotopic composition should be sourced and supplied to all
participants. The availability of samples from the recent IAEA proficiency testing
progamme (WICO) will be investigated.
5) The possibility of purchasing and distributing other reference materials should be
investigated. These may be:
a. Whole Milk Powder (NIST 1549a) trace elements
b. Skimmed Milk ERM-BD150 trace elements
c. Skimmed Milk ERM-BD151 (spiked) trace elements
d. IAEA 152 Dairy (Out of stock) Isotope values, not certified (C, N and H)
6) A casein standard should be developed. A bulk (5-10 kg) amount of casein will be
purchased from a chemical supplier. This will be homogenized and subsampled at the
IAEA for distribution to participants. No analytical values will be available for this
initially. It will be used as a quality control (QC) material until sufficient information
is available to assign values for H, C, N, O, S, Sr isotopes and trace elements.
7) Recommend to FIRMS and FIT-PTS Milk Powder as a material for interlaboratory
trials.
8) IAEA should coordinate the 1st interlaboratory trials of reference materials including
Casein.
9) The results of the 1st interlaboratory trials should be presented at a special session of
the Food Safety and Traceability Conference in Vienna, Nov. 2014 (potential venue
for a training workshop and feedback session for the CRP participants).
6 6
10) A book should be prepared that compiles the accepted procedures for sampling and
stable isotope analysis of milk. This will be produced as a resource for the participants
and later for all member states.
11) All participants should communicate regularly. To help facilitate communication, a
website for deposit of information with a forum for discussion was set up during the
meeting.
12) Statistical methods training should be incorporated into the programme of activities.
This will include on-line tutorials and a session added to a future Coordination
meeting.
7 7
Agreed Work Plan and Logical Framework
Work Plan (Activities)
Activity 2013 2014 2015 2016 2017 2018
CRP advertised (March 2013) and research contract
and agreements awarded.
Contracts and agreements signed by end November
2013.
X
1st RCM, Vienna (26
th to 29
th November 2013) agreed
CRP strategy and research work plans.
X
Awarded Research Contracts X
Phase 1: 18 months’ work programme completed. X
Prepare book with guidelines for sampling and
analysis of milk
Draft
by Q2
2nd
RCM (May 2015) to be held in Morocco (subject
to Host country and IAEA approval) to review the
work conducted in Phase 1 based on progress reports
and presentations. Detailed work plans for Phase 2
agreed to ensure that the CRP objectives are met.
Q2
Phase 2 : Work programme
Organise 3rd
RCM (Q4 2016) to review work
conducted in Phase 2 and agree final phase 3 work
programme.
(Proposed Venue: Singapore. This is subject to Host
country and IAEA approval).
Phase 3: Work programme
Final RCM: (Q1 2018) to review Phase 3 work and
prepare a TECDOC and /or research papers to an
appropriate journal.
Assumptions
(a) Submissions will be received from suitable laboratories with qualified staff, access
to appropriate techniques, equipment and experience.
(b) Participants have budgetary support for activities not funded by the CRP (staff
resources, instrumentation and maintenance costs).
8
Annex I: RCM Attendees
Agreement Holders
Jurian HOOGEWERFF
University of Otago
P.O.Box 56, Dunedin 9016
NEW ZEALAND
Barry Thornton
The James Hutton Institute
Craigiebuckler
Aberdeen AB15 8QH
Scotland
UNITED KINGDOM
Jose Almirall
Florida International University
Department of Chemistry and Biochemistry
FL 33199 MIAMI
UNITED STATES OF AMERICA
Gabriel Bowen
1620 Wasatch Dr.
SALT LAKE CITY
UT 84108
UNITED STATES OF AMERICA
Contract Holders
Daniel Wunderlin
Universidad Nacional de Córdoba
Obispo Trejo 242
X5000IYF Córdoba
Pcia. de Córdoba
ARGENTINA
Gang Chen
Chinese Academy of Agricultural Sciences
CAAS - IQSTAP
12 Zhongguancun Nandajie
South Road P.O. Box 5109
BEIJING 100081
CHINA
Khaled EL Hawari
Lebanese Atomic Energy Commission (LAEC)
National Council for Scientific Research (CNRS)
P.O.Box 11-8281
Riad EL Solh 1107 2260 ,Beirut
LEBANON
Andrius Garbaras
Center for Physical Sciences and Technology
Savanoriu ave. 231
LT-02300 VILNIUS
LITHUANIA
Noureddine Amenzou
Centre national de l'énergie, des sciences et des
techniques nucléaires (CNESTEN)
B.P. 1382, route principale
RABAT AGDAL 10001
MOROCCO
Ryszard Wierzchnicki
Institute of Nuclear Chemistry and Technology
ul. Dorodna 16
03-195 Warsaw
POLAND
9 9
Ivan Vladimirovich Podkolzin
Federal Centre for Animal Health
600901, Vladimir
Yur’evets
RUSSIAN FEDERATION
Shirley Suat Lay Chua
Veterinary Public Health Laboratory
Microbiology Department
Laboratories Group
Agri-Food and Veterinary Authority
10 Perahu Road
SINGAPORE 718837
Nives Ogrinc
Department of Environmental Sciences
Reactor Centre; Jozef Stefan Institute
P.O. Box 3000, Jamova 39
LJUBLJANA 1001
SLOVENIA
Preeni Abeynayake
Department of Veterinary Public Health &
Pharmacology
Veterinary Medicine and Animal Science
University of Peradeniya
Peradeniya (20400)
SRI LANKA
Observers
Joanne Sheot Harn Chan
Food Safety Division - Applied Sciences Group
Health Sciences Authority
11 Outram Road
SINGAPORE 169078
Micha Horacek
HBLFA Francisco Josephinum
Weinzierl 1
3250 Wieselburg
AUSTRIA
Rebecca Hood-Nowotny
rebecca.clare.hood-
Department of Terrestrial Ecosystem Research
University of Vienna
Althanstrasse 14
1090 VIENNA
AUSTRIA
IAEA
Mr Russell Frew
Food and Environmental Protection Laboratory
International Atomic Energy Agency
Vienna International Centre, PO Box 100,
1400 Vienna, Austria
Mr Andrew Cannavan
Food and Environmental Protection Laboratory
International Atomic Energy Agency
Vienna International Centre, PO Box 100,
1400 Vienna, Austria
Ms Zora Jandric
Food and Environmental Protection Laboratory
International Atomic Energy Agency
Vienna International Centre, PO Box 100, 1400 Vienna, Austria
Apologies: Ms Roksana Huque (Bangladesh, Contract No. 18195) was not able to attend.
10 10
Annex II: Meeting Agenda
26 – 29 November 2013
IAEA Vienna, Austria
Room C5
CRP Technical Officers: Russell Frew ([email protected])
Andrew Cannavan ([email protected]);
Administrative secretary: Kyoko Viitaniemi ([email protected])
Provisional Agenda
Day 1: Tuesday, 26 November 2013
08:30 Registration, UN Pass Office, Gate 1, Vienna International
Centre
All
09:30 Welcome & Opening Address Andrew Cannavan, IAEA
09:45 Introduction and Presentation of Participants All
09:55 Election of Chairperson and Adoption of Agenda All
10:00 CRP background: objectives and scope of the RCM in line with
the conclusions and recommendations from consultants meeting
Russell Frew, IAEA
10:20 Break – Participants to do banking
Session 1: Contract Holder Presentations (Proposed Research work plan, summary of work done to
date and future work plan meeting the objective of the CRP)
11:00 Daniel Wunderlin, Argentina:
11:30 Gang Chen, China
12:00 Lunch / Administrative Arrangements
Contract Holder Presentations (Proposed Research work plan, summary of work done to date and
future work plan meeting the objective of the CRP)
14:00 Shirley Suat Lay Chua , Singapore
14:30 Preeni Abeynayake: Sri Lanka
15:00 Khaled El Hawari, Lebanon:
15:30 Break
15:45 Andrius Garbaras, Lithuania:
16:15 Noureddine Amenzou, Morocco:
16:45 Ryszard Wierzchnicki, Poland:
17:15 Closing remarks
17:30 Wine and cheese
11 11
Day 2: Wednesday 27th
November 2013
08:30 Summary of Day 1 Andrew Cannavan,
Russell Frew
08:45 Ivan Vladimirovich Podkolzin, Russian Federation:
09:15 Nives Ogrinc, Slovenia:
09:45 Micha Horacek, Austria
10:15 Break
10:45 Gabe Bowen, USA
11:15 Jurian Hoogewerff, New Zealand
12:00 Lunch
Session 2: Presentations from Agreement Holders
13:45 Barry Thornton, United Kingdom
14:15 Jose Almirall, USA
14:45 Zora Jandric, IAEA
15:00 Break
Session 3: Preparation of Work Plans, Recommendations and Meeting report
15:15 Discussion of work plans: Formation of work groups (led by
Agreement Holders) to put together detailed work plans during
Session 3
All
16:45 Formation of working groups
Group 1: Core Isotopic Assays
Group 2: Supplementary Techniques applicable for food
traceability
Chairperson and
Agreement Holders
17:30 End of Day 2
Day 3: Thursday 28th
November 2013
08:30 Summary of Day 3 Russell Frew, Andrew
Cannavan,
8:45 Brainstorming Session 1: to identify tasks for the 2nd
year of
the project.
The tasks may include comparative assessment; benchmarking;
exchange of data; cooperation in method development, etc.
The outputs of this session are expected to be written
suggestions for certain tasks to be performed by participants of
each group.
All
12 12
10:30 Break
10:45 Brainstorming Session 1 (continued) All
12:30 Lunch Break
14:00 Drafting Session 1. The objective of this session is to prepare
presentations (one for each group) of the findings of
Brainstorming Session 1
Agreement Holders and
participants of groups
15:30 Break
16:00 Presentation of Group 1, Q&A Chairperson of Group 1
16:30 Presentation of Group 2, Q&A Chairperson of Group 2
17:00 Discussion on outcomes of Brainstorming Session 1 All
17:30 End of Day 3
Day 4: Friday, 29th
November 2013
08:30 Summary of Day 3 Russell Frew, Andrew
Cannavan,
08:45 Drafting Session 2. The objective of this session is to
prepare a consistent write-up of the findings of
Brainstorming Session 1 (i.e. work plans for the next phase
of the project)
All
10:00 Review the written reports of the working groups. All
10:30 Break
10:45 Brainstorming Session 2. The objective of this session is
to define the number, the titles, the scope and the structure
of Reports to be produced within this CRP, by each
Contract Holder and cumulatively.
The suggestions are expected to be based on the outputs of
Brainstorming Sessions 1
All
12:30 Lunch
14:00 Drafting Session 3. The objective of this session is to
prepare a consistent write-up of the proposals of
Brainstorming Session 2
All
15:15 Break
15:30 Review the outputs of Drafting Session 3 All
16:00 Discussion on the conclusions and recommendations of the
meeting (the draft will be prepared by the scientific
secretary and distributed prior to this session)
All
17:00 Finalizing conclusions and recommendations All
17:30 Closing Remarks and End of Meeting
13
Annex III: Analytical Methods and Programme Capabilities
• Whole Milk (Proxies –water and Casein) by H, O in liquid and C, N in Casein
• Milk Powder (Solid), C, N, H, O and Sr
• Milk Powder (major, minor and trace elements) solution/digestion ICP-MS, LA-ICP-
MS, XRF, LIBS
• Casein (major, minor and trace elements) solution/digestion ICP-MS, LA-ICP-MS,
XRF, LIBS
Complimentary analyses
• Milk Powder (small molecule analysis), Fatty Acids, Amino acids
Capability Within Project
• Stable Isotopes
C/N – Argentina, Lithuania, Poland, Slovenia, Russia, Morocco, UK,
Singapore, China, Lebanon (C only), NZ
CRS (C/H), Lebanon, UK
H/O (water) –Lithuania, Poland, Slovenia, Lebanon, Argentina, Morocco, UK,
China, NZ
H (solid) – Lithuania, Lebanon, UK, Singapore, China, NZ
Sr – Lithuania, Poland, Argentina, Morocco, UK, USA, NZ
• Major, Minor and Trace Elements
ICP-MS - Lithuania, Slovenia, Russia, Argentina, Morocco, UK, Singapore,
China, NZ
LA-ICP-MS - Lithuania, Singapore, USA, NZ
XRF - Slovenia, UK, USA,
LIBS - USA
• Small molecule analysis (Fatty/Amino Acids)
GC-MS - Argentina, Slovenia, Lebanon, China, Poland, UK, NZ
LC-MS - Argentina, Lithuania, Morocco, Singapore, UK
14
Annex IV: Background and Metadata Guidelines
Background – Summarize information on major producers
o Geographic location (lat/long, decimal degrees, +/-)
o Elevation (meters above sea level)
o Spatial footprint – where is the milk collected from (narrative/text)
o Number and size of individual farms
o Total production volume (L/day)
o Production type (milk powder/cheese/condensed milk/milk distributor)
o Farming practices
Dominant breed (Fresian/Jersey/Brahim/Zebu/Holstein/other)
Feeds used (pasture/ supplements/hay/silage/other)
Pastured/housed/mix
Dominant water sources (GW/SW/distinctive characteristics)
o Distinctive regional conditions (local urban areas, land use legacy, ecoregions;
narrative)
o Local climate station available?
o Geological map available?
o Soil map available?
o Closest precipitation isotope station (can be filled after the fact)
Metadata
o Sites
Site ID
Geographic location (lat/long, decimal degrees, +/-)
Elevation (meters above sea level)
Facility name
Facility type
o Samples
Sample ID
Site ID
Date of collection (Date)
Time of collection (Time)
Unit of collection (cow/farm/collecting station or plant)
Cow ID (optional)
Water sample collected?
Soil sample collected?
Feed sample collected?
15 15
Annex V: Report from Sampling Workgroup
Major questions
o Will we better be able to distinguish between major regions/nations or
between farms w/in regions?
o Which questions are more relevant?
o Starting point characterize chemical variability within, between regions and
relationship w/ environmental drivers
What secondary effects that might influence isotopes and chemistry of products?
o Are there differences related to breed?
o Are there effects related to additives/fortifiers?
o What is the influence of feeding system?
Whole vs. powder milk
o Do producers specialize on one or the other?
o Whole milk most general, flexible, biggest bang for buck (both solids and
water)
o How do we sample whole milk in a way that aggregates variability in the same
way as powder?
Task: inventory/map major dairy facilities (whole milk aggregators, power producers)
o Compile as much information as possible on characteristics and practices
(what products, how much, catchment area, rearing practices, watering
regimes)
o Produce common spreadsheets w/ info for each region, share, and push to map
How many samples?
o 3 x per year sample from any given producer
o Aim to collect at least 50 samples per year
How much emphasis on sampling product vs. sampling environment
o Start with emphasis on product to characterize modes of variability?
o Monthly precipitation sampling…need protocol, based on NZ experience
o Soil to be sampled for elements, bulk organic H in some cases but not all?
o Fertilizer samples for N in some cases?
Where to get samples – authentics vs. point-of-consumption
o Can each group try to develop relationships to collect some authentics?
o Scales – farm, industry, commercial product
o Activity: comparing authentics with commercial samples from same producer
Should we collect commercial samples at same time as authentics for
subsequent comparison?
Sample handling protocols required
o Rain water – in hand
Need to get samples analyzed in reasonable time
o Whole milk – develop protocol that is feasible for all/most participants
Prefer freezing to refrigeration, leave headspace in bottles
Separation of water from solids via cryogenic distillation (Daniel to
test that this is comparable w/ sprayer)
16 16
De-fatting, save fat fraction
Process ~150 - 200 ml to get ~15 - 20 g solids (use 150 ml Nalgene
HDPE bottles?)
o Soil sampling and handling – in hand
Sample metadata
o Geographic
o Temporal
o Environmental
o Producer/supplier
o Sample codes
o Compositional information from producer
IAEA supports the database?
o Who will do this w/in the agency?
o Longevity?
17 17
Annex VI: Work plans 1st Phase January 2014 to June 2015.
Country: Argentina Contract No. 18059
Project Title Ensuring the origin and safety of Argentinean milk.
Lead Partner Prof. Dr. Daniel A. Wunderlin
Start month Jan 2014
End month Dec 2014
Interaction with other partners Yes
Technical support required Yes
OBJECTIVES
Main Objective: Demonstrate the usefulness of combined techniques (TE + isotopic fingerprint) to predict the origin of dried milk and the influence of diverse feeding and environmental conditions on this fingerprint.
Specific Objectives: a) To verify SOPs for measuring TE and stable isotopes (light and heavy) in agricultural
soil, forage, water and milk (dried). Evaluation of LODs LOQs, accuracy, QA-QC parameters, etc.
b) To measure TE and stable isotopes in CRMs and also in samples (soil, water, forage and dried milk)collected from diverse regions belonging to the main milk producing area of Argentina (Provinces of Santa Fe and Córdoba). Thus, analyzing authentic samples with dried milk produced in the laboratory.
c) To evaluate elements-isotopes within the TE+ isotopic fingerprint, allowing to differentiate milk from diverse regions using chemometrics to evidence which parameters are the most important to point out such differences.
d) To verify the matching between soil-water-forage and milk composition using appropriate multivariate correlations (canonical correlation analysis (CCA), Generalized Procrustes Analysis (GPA), etc.).
e) To compare our results with results from other latitudes looking for a generalized model that could be expanded to other countries, continents, verifying the scope of developed methods to predict the origin and, if possible, the safety of dairy products.
DESCRIPTION OF WORK
Task 1: Sampling
During the first year samples will be taken considering temporal and spatial variations by personnel belonging to the National Institute for Agricultural Technology (INTA, Rafaela, Province of Santa Fe).
Soil samples will be collected once from 6 farms distributed in Provinces of Santa Fe and Córdoba, completing at least four independent soil samples from each farm (n= 24).
Water samples will be collected twice from 6 farms distributed in Provinces of Santa Fe and Córdoba, considering rainy and drought periods (one sampling during each period), completing at least two independent water samples from each farm at each period (n= 24: 12 from rainy season and 12 from dry season).
Forage and whole fresh milk samples will be collected during four seasons (winter, spring, summer and autumn) from 6 farms distributed in Provinces of Santa Fe and
18 18
Córdoba (one sampling during each period), completing at least two independent forage samples from each farm at each period (n= 48: 12 from each season). Milk will be dried at the laboratory (INTA-Rafaela, Santa Fe, Argentina) using a spray drier (Büchi, Swiss) and conditioned in plastic containers.
Samples will be conditioned in INTA and submitted for analysis to the Institute for Food Science and Technology (ICYTAC, Córdoba, Argentina), in charge of sample preparation and analysis.
Task 2: Analysis
Trace elements (TE): 30+ elements will be determined in each sample considering protocols developed during our participation in the TRACE project and recent publications (Podio et al., 2013, Baroni et al., 2011).
Isotopic analyses: Light isotopes (δ2H, δ13C, δ15N, δ18O) will be measured at INGEIS (CONICET-UBA, Buenos Aires, Argentina) in according to protocols developed during our participation in the TRACE project and recent publications (Podio et al., 2013; Baroni et al., 2012). Heavy isotopes (87Sr/86Sr) will be measured by TIMS at CONEA (Buenos Aires Argentina) with sample preparation at INGEIS (Buenos Aires, Argentina) using protocols developed during our participation in the TRACE project and recent publications (Podio et al., 2013; Baroni et al., 2011). Some samples will be sent to partners for comparasion and analysis of some elements not availables at our lab.
Xenobiotic and VOCs analyses (conditioned to obtaining additional support, grants, etc.). Analysis of pesticides and veterinary drugs (antibiotics, etc.) will be performed by GC-MS or HPLC-MS/MS, using protocols recently published by the group (Bonansea et al., 2013). Analysis of toxins will be performed mainly by HPLC coupled to MS or MS/MS in according with recent experience from the group (Galanti et al., 2013).
Task 3: Data mining
Statistics-Chemometrics: Results arising from chemical-isotopical analysis will be analyzed using multivariate
methods, namely principal components (PCA), cluster analysis (CA), Discriminant Analysis (DA), Generalized Procrustes (GPA), Canonical Correlation (CCA) and other statistical methods when necessary. All these methods have been fitted during our recent work to establish differences between samples from diverse provenance, pointing out main parameters necessary to verify such differences. Additionally, these methods allow matching the composition of different matrixes (soil, water, forage and milk), establishing correlations between the geology, hydrology, plant chemistry and the follow up to the milk (Podio et al., 2013; Baroni et al., 201). In addition to discrimination from sample provenance, we will look to verify the influence of diverse environments / pollution. Methods to be used will be the same described above but grouping samples in according to other criteria (e.g. presence / absence of xenobiotics; major / minor presence of toxic compounds in the environment (soil, water, forage, etc.)). These last analyses should allow evidencing markers (chemical or isotopes) of environmental pollution (if any) translated to the milk from soil, water or forage. Additionally, markers (chemical or isotopes) of different feeding could be found using these statistical techniques to groups of samples arising from cows receiving different type of forage (field grass, silage grass, silage maize, etc.).
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Task 4: Write and send an annual report to be evaluated by IAEA scientific board.
DELIVERABLES
No. Description Month
1 Inter-laboratories comparison for TE + Isotopes 1-6
1 Samples processed, ready to analysis 6-12
2 TE analysis 6-12
3 Isotopic analysis 10-12
4 Statistical analysis 12
5 Report 12
6 Peer reviewed publications 12+
EXPECTED RESULTS
Expected Outputs:
1) Peer reviewed publications containing main findings from the proposed study, results from round Robin tests, etc.
2) Scientific-Technical report to IAEA-FAO, pointing out analytical methods and statistical tools necessary to ensure milk provenance, considering diverse regions, environments and feeding. Special attention will be paid to chemical-isotopic markers pointing out risks associated with the production of milk in non-safe areas (not clean, polluted) or the presence of toxic products (veterinary drugs, toxins, pesticides, etc.).
3) Presentation of results at specialized scientific meetings to spread acquired knowledge between the community dedicated to the study of food safety, traceability, etc.
4) Presentation of results to policy makers to influence future decisions on quality assurance and quality control of dairy products in view of results obtained from the present study.
20 20
Country: P.R. China Contract No. 18057
Project Title Stable Isotopes and Chemical Contaminants
Analysis to Trace the Origin and Safety of Dairy
Milk in China
Lead Partner Gang Chen
Start month Jan 2014
End month Dec 2014
Interaction with other partners
Technical support required
OBJECTIVES
♣ To establish a powerful tool to trace the milk products origin and authenticity, and find
contaminants early enough before they spread and cause social panic.
♣ The established tracing system will also help to improve the market surveillance, protect
quality and safety of products as well as resume the trust and rejuvenate the Chinese
dairy industry.
♣ Furthermore, implementation of the project will gain experience on establishing the
tracing system on other food products, and ensure the food safety from a much wider
perspective.
DESCRIPTION OF WORK
Task 1: delineate the milk production area on the map. Make work plan. Decide the sampling area.
Check the geological information of the area. Prepare questionnaire, protocol etc.
Task 2: finish the proficiency test samples before the end of February. The analysis include C/N/H/O.
Task 3: contact farmers for sampling. Samples include whole milk, water and soil.
Task 4: The method for simultaneous melamine and cyanuric acid analysis in dairy milk will be
established by using liquid chromatography mass spectrometry (LC-MS/MS). Deuterium
labeled references will be spiked as internal standard. The method validation procedure will
follow the EU Commission Decision (2002/657/EC). The sensitivity will below 10 μg/kg.
Task 5: The estrogens targeted include estrone, α-estradiol, β-estradiol, and estriol. Deuterium labeled
internal standards will be used. Samples will be derivatized by dansyl chloride (DNS-Cl) to
improve sensitivity. In order to remove the matrix effect and the contamination of DNS-Cl
regent to LC-MS/MS ion source, an on-line solid phase extraction procedure will be established
for sample cleanup. The sensitivity of developed method will reach 1 pg/g.
Task 6: The collected real milk samples will be analyzed for the above chemicals.
Task 7: Write and send an annual report to be evaluated by IAEA scientific board.
DELIVERABLES
No. Description Month
1 Delineate the sampling area in Chinese map End of December, 2013
2 Assemble the freeze drier for distilling water from whole
milk
End of June, 2014
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3 Proficiency test (bulk milk) End of February, 2014
4 Sampling in certain area Until March, 2015
5 Finishing the core analysis (C/N/H/O) in defatted milk and
soil. H/O in water
End of October, 2014
6 Submit annual report Beginning of November, 2014
EXPECTED RESULTS
1. Overview of the milk production in China, make a milk map for further sampling.
2. Sampling as much as possible following a protocol provided in the group.
3. Platform establishment, such as water distillation with freeze drier, etc. In order to achieve this, the
detailed protocols are highly required.
4. Get preliminary stable isotopes data in milk samples.
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Country: Lebanon Contract No. 18044
Project Title Study of regional and seasonal variation in fatty
acid composition and stable isotopes of milk
produced in Lebanon
Lead Partner
Start month Jan 2014
End month Dec 2014
Interaction with other partners
Technical support required Protocols for stable isotopes sample preparations
OBJECTIVES
The research project is address to study the variations of isotopic enrichments (Carbon and
Hydrogen) and fatty acids of milk produced in Lebanon and collected from different
geographical locations and season of the year. Cavity ring down spectroscopy and gas
chromatography are respectively used for the determination of light stable isotopes (carbon and
hydrogen) and fatty acids. The objective for the first year is to have analytical method that able
to analyse δ2H stable isotope in water milk and δ
13C in casein and whole milk using cavity ring
down spectroscopy (PICARRO B2221-I) and to ensure the reliability of results through
conducting inter-laboratory comparison of reference material and laboratory samples
DESCRIPTION OF WORK
Task 1: Purchase cryogenic distillation apparatus to separate water milk from raw milk based on G.
West et al. (2006) approach for the determination of δ2H
Task 2: Purchase certified reference material (IAEA-600, IAEA-CH-7, GISP, and IAEA-152 (if
available)) and Picarro consumables and spare parts
Task 3: Develop then validate analytical method to extract milk water and casein from milk using
cryogenic distillation and freeze dryer followed by CRDS analysis after being calibrated
Task 4: Participation into inter-comparison laboratory testing for the determination of δ2H and δ
13C for
RM and purified casein then evaluate our results
Task 5: Collect information’s about farms location in Lebanon taking into count major production areas
and their location
Task 6: Start method development for fatty acid in milk using GCMS
Task 7: Write and send an annual report to be evaluated by IAEA scientific board.
DELIVERABLES
No. Description Month
1 Purchase cryogenic distillation apparatus (2-3 months)
2 Purchase CRM and Picarro consumables (2-3 months)
3 Develop analytical method for stable isotopes (2 months)
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4 Participation into inter-comparison (1 month)
5 Method development of fatty acids on GCMS (4 month)
6 Collecting information’s about farms (1 months)
EXPECTED RESULTS
Depending on the results getting form inter-laboratory testing for δ2H and δ
13C in milk we are expecting
to have a validate method for the analysis of stable isotope in our laboratory using cavity ring down
spectroscopy unless we need to optimise our methodologies to get comparable isotopic values which are
obtained from EA-IRMS.
24 24
Country: Lithuania Contract No. 18069
Project Title Accessible Technologies for the Verification of
Origin of Dairy Products as an Example Control
System to Enhance Global Trade and Food Safety
Lead Partner Center for Physical Sciences and Technology
(CPST)
Start month Jan 2014
End month Dec 2014
Interaction with other partners
Technical support required
OBJECTIVES
DESCRIPTION OF WORK
Task 1: Data collection about the producers of the dairy products in Lithuania
Task 2: Implementation of the milk and water samples collection techniques
Task 3: Collection of the dairy products and water in Lithuania
Task 4: Analysis of C, N, O, H isotopes in milk, milk powder and water (only H and O)
Task 5: Participation in the interlaboratory comparison
Task 6: Construction of the cryogenic distillation system
Task 7: Write and send an annual report to be evaluated by IAEA scientific board.
DELIVERABLES
No. Description Month
1 Interlaboratory comparison: C, N in the milk powder 2014 01- 02
2 Collection of water and dairy products 2014 01 -
3 Analysis of the samples 2014 02 -
4 Manuscript on methodology about whole milk H an O
analysis (optional)
2014 09
5
6
EXPECTED RESULTS
Data on C, N, H, O isotopes in the dairy products and water in Lithuania
Manuscript on the method for the milk H and O analysis
25 25
Country: Morocco Contract No. 18051
Project Title Stable isotope ratios and trace elements in Dairy
Products (Milk and cheese) as new tool to
determine their different origins in Morocco
Lead Partner Office National de la Sécurité Sanitaire des
Produits Alimentaires-ONSSA-(Food Safety
Agency) Start month Jan 2014
End month Dec 2014
Interaction with other partners 1 : National Association of goats and sheep
(ANOC) http://www.anoc.ma 2 : Association Nationale des Eleveurs de Bovins
(ANEB)
Technical support required Standards materials for stable isotopes analysis
OBJECTIVES:
- Training in analytical techniques for this purpose, including implementation of quality
systems, reference materials, reporting procedures ;
- Test of isotopic techniques (13
C/12
C, 15
N/14
N, 18
O/16
O, D/H, 87
Sr/86
Sr) and trace elements in
milk and cheese in the order to determine the geographic origin of dairy products in
Morocco.
- Realization of map distribution of milk in Morocco
- Help the national authority for the determination of food origin
DESCRIPTION OF WORK
Task 1: Preparation of reference material, and procedure for analysis and Proficiency test
Task 2: Collecting of background information (soil, and climatic data, milk production, farmer practice
….) in order to determine of sampling sites
Task 3: Collecting of milk, soil water and feed samples
Task 4: Preparation samples
Task 5: stable isotopes (C, N, O), strontium ratio and traces elemental analysis
Task6: statistical (multi - variate) treatments and interpretation of results
Task 7: Write and send an annual report to be evaluated by IAEA scientific board
DELIVERABLES
No. Description Month
1 Reference material, procedure of analyses and Proficiency
test
Jan-feb 2014
2 Sampling map Mar 2014
3 Sampling report and samples Apr - May 2014
4 Results of all analysis Jul - July 2014
5 Statistical treatment Sept 2014
6 Interpretation and writing report Oct – Dec 2014
EXPECTED RESULTS
- Procedure of stable isotope and trace element analyses
- National database of isotopic composition and trace elements concentrations of dairy products.
- Maps containing the spatial and temporal variability of the isotope signature of dairy products
across Morocco.
26 26
Country: Poland Contract No. 18056
Project Title The study of the Influence of the Environmental
Factors on the Isotopic Composition of Dairy
Products
Lead Partner Institute of Nuclear Chemistry and Technology,
Warsaw, Poland
Start month Jan 2014
End month Dec 2014
Interaction with other partners Warsaw University of Life Sciences – SGGW
(Faculty of Food Sciences)
Technical support required Methods description, protocols
OBJECTIVES; Influence of environmental factors on the isotopic composition of milk as a way to
global traceability system for dairy products.
DESCRIPTION OF WORK
Task 1: Selection of regions for the study (sampling)
Task 2: Elaboration of sampling method for milk and for environmental samples (soil)
Task 3: Collection of authentic samples of milk (June – September)
Task 4: Chemical methods for separation of some chemical components of environmental samples
Task 5: Measurement of isotopic composition of N,C and Sr
Task 6: Statistical methods for isotopic results elaboration.
Task 7: Write and send an annual report to be evaluated by IAEA scientific board.
DELIVERABLES
No. Description Month
1 Results of 1 round interlaboratory comparison February
2 Results of 2 round interlaboratory comparison April
3 Results of 3 round interlaboratory comparison June
4 Map of regions and net of sampling points March
5 Results of isotopic parameters of soil samples November
6 Results of 1st year measurements of milk December
EXPECTED RESULTS Mathematical correlations between isotopic composition of milk and
isotopic composition of some elements of environment like a rainwater, grass and soil.
27 27
Country: Russian Federation Contract No. 18096
Project Title Accessible Technologies for the Verification of
Origin of Dairy Products (D52038)
Lead Partner
Start month Jan 2014
End month Dec 2014
Interaction with other partners
Technical support required Data Analysis performing MV statistical procedures
OBJECTIVES
Implementation of scientific approaches for identifying origin of dairy products
DESCRIPTION OF WORK
Task 1: Collect the information about milk producers within the country.
Task 2: Purchase silver capsules for O/H determination (solid phase).
Task 3: Purchase appropriate standards and reference materials to execute proficiently test.
Task 4: Preform and validate the method for C,N,O,H determination.
Task 5: Sample collection.
Task 6: First measurements and interim results.
Task 7: Start to development GC-IRMS method for determination of some compounds of milk.
Task 8: Write and send an annual report to be evaluated by IAEA scientific board.
DELIVERABLES
No. Description Month
1 Purchase silver capsules for O/H determination (solid
phase).
2 months (Dec 13 - Jan 14)
2 Collect the information about milk producers within the
country.
1 month (Jan 2014)
3 Purchase appropriate standards and reference materials to
execute proficiently test.
2-3 months (until Feb 2014)
4 Preform and validate the method for C,N,O,H
determination.
Approx. 4 months (Jan - Apr)
5 Sample collection 10 months (Jan - Oct)
6 First measurements and interim results. 7 months (Mar - Oct)
7 Start to development GC-IRMS method for determination
of some compounds of milk.
Approx. 3 (Feb – Jun)
8 Summary Report 1 month (Oct – Dec)
EXPECTED RESULTS
Having comprehensive information about samples
Having Ready to use methods for determination of common stabiles isotopes C, N, H, O.
First edition of Standard operating procedure
Data acquisition and preparation the ground for the creation of database
28 28
Country: Singapore Contract No. 18070/R0
Project Title To Establish Methods for the Detection of Adulteration
and Provenancing of Milk and Milk Products Using
Stable Isotope Signatures, Trace Elements Analyses,
Chromatographic and Spectroscopic Techniques.
Lead Partner Agri-Food & Veterinary Authority of Singapore
Start month Jan 2014
End month Dec 2014
Interaction with other partners Health Sciences Authority
Technical support required Reference Materials and Protocols for sampling and
stable isotope analysis
OBJECTIVES
To install a workflow using techniques for the measurement of various stable isotopic signatures and
trace elements in the milk and milk products to assess their discriminatory power for source
tracing/provenancing as well as their ability to detect suspected presence of adulterants, which can then
be subjected to further analysis, such as chromatography, for confirmation of identity. DESCRIPTION OF WORK Task 1: Participate in inter-laboratory comparison among member countries
Task 2: Establish a QC material for AVA and HSA.
Task 3: Establish work flow for the collection and documentation of liquid milk (and if possible water,
feed and soil) from local dairy farm and imports from major markets.
Task 4: Establish protocols for sampling. Sampling plan to take into consideration seasonal variations
(x3 samples/month/farm or x3 samples/quarter/import brand). Sample collection. Task 5: Establish methods for samples preparation and instrumental analysis (C, N, O, H)
Task 6: Validation of methods for sample preparation and instrumentations if possible.
Task 7: Cross validation of methods established between AVA and HSA
Task 8: Analysis of samples (?)
Task 9: Write and send an annual report to be evaluated by IAEA scientific board.
DELIVERABLES
No. Description Month
1 Participation in inter-laboratory comparison among member
countries
Jan-Feb 2014
2 Establish a QC material for AVA and HSA. Mar – Jun 2014
3 Protocols for sampling. On-going starting from Jan 2014
4 Documented workflow for collection and documentation of
liquid milk (and if possible water, feed and soil) from local
dairy farm and imports from major markets.
March 2014 – Mar 2015
5 Standard Operating Procedures for the validation of
methods for sample preparation and instrumentation.
Validation of stable isotope methods for sample
preparation and instrumentations if possible.
Feb - Aug 2014
6 Summary Report Oct 2014 EXPECTED RESULTS
Standard Operating Procedures and/or protocols for the following: • Collection and documentation of liquid milk available in the market • Sampling of liquid milk products • Validated methods for sample preparation and instrumentation • Validated methods for routine analysis of liquid milk products for provenance and adulteration
testing in Singapore (and which may be extended to other countries in the region)
29 29
Country: Slovenia Contract No. 17897
Project Title The use of stable isotopes and elemental
composition for determination of authenticity and
geographical origin of milk and dairy products
Lead Partner Jožef Stefan Institute, Slovenia
Start month Jan 2014
End month Dec 2014
Interaction with other partners Dairy producers
Technical support required Inter-laboratory comparision
OBJECTIVES
The overall objective of the proposed project is to use the isotopic and elemental composition in order to
determine geographical origin of Slovenian milk. Slovenia is a small country regarding surface area, but
pedologically and climatically diverse, and thus it offers an ideal area for studying the natural factors
which govern the isotopic distribution in milk and its products.
This general objective can be broken down to four more specific objectives that would together achieve
the overall goal of the project as follows:
• to construct the database on the elemental and isotopic composition of Slovenian milk;
• to perform statistical evaluation of the data and thus select parameters important for determination
of geographical origin of Slovenian milk;
• to develop the system for monitoring of food products and methods for the control of food such as
milk and its products;
• to establish the system for food traceability that could be transferred to other countries (including
developing countries) and other commodities.
DESCRIPTION OF WORK
Task 1: Purchase of additional certified reference material (IAEA600 caffein). Perform all possible
analysis on reference material (stable isotope analysis, trace elements, fatty acids), casein, UHT-milk.
Task 2: Participation in the inter-laboratory comparison between CRP partners
Task 3: Writing the SOP for stable isotope analysis on dairy products
Task 4: Perform the data for meta-database, background information according to the spreadsheet
available
Task 5: The sampling of milk will be performed every month covering different geographical regions
(Mediterranean, Pannonia, Dinaric and Alpine) in Slovenia. Samples will be provided by five Slovenian
diary producers (Ljubljanske mlekarne, Pomurske mlekarne, Vipavske mlekrane, Mlekarna Planika and
Mlekarna Celeia). The samples will be stored at −20oC before analysis. The isotopic composition of O
will be determined monthly, while the isotopic composition of N and C in casein and multi-elemental
composition will be determined seasonally in March, June, September and December. Ancillary data
(soil and feeding) will be also provided. Check about milk powder.
Task 6: Evaluation of the data – statistical evaluation, modeling
Task 7: Write and send an annual report to be evaluated by IAEA scientific board.
DELIVERABLES
30 30
No. Description Month
1 Obtained appropriate CRM 1-2
2 Results on the inter-laboratory comparison 2
3 SOPs 6
4 Data base on background information on sampling sites 2
5 Data on the O, H in milk water, C, N in casein, major and
trace elements and fatty acid composition
12
6 Evaluation of the data + presentations + publication 15
7 Annual IAEA report 18
EXPECTED RESULTS
The main output of the project is the construction of authentic comparative database of Slovenian milk
including stable isotope and elemental composition. In the long-term the generation of isotopic and
multi-element maps of foods from different geographical locations could be constructed and
incorporated intro traceability systems. The work will be presented at workshops to national and
international communities and published in international recognized journals.
The results of the proposed project will be important for scientific and social-economic development and
will enable efficient exchange of new knowledge and incorporation in new food studies. The proposed
project includes a combination of different analytical techniques and approaches that will contribute to
the establishing and updating of large-scale databases and made a scientific basis for the development of
new approaches that could be included in new regulations. The proposed approaches will strengthening
the competitiveness of the whole agro-food chain and at the same time protect the consumer and good
name of the country.
31 31
Country: Sri Lanka Contract No. 18066
Project Title Accessible Technologies for the Verification of
Origin of Dairy Products as an Example Control
System to Enhance Global Trade and Food Safety
Lead Partner Ms Champa Dissanayake
Start month Jan 2014
End month Dec 2014
Interaction with other partners Preeni Abeynayake, Faculty of Veterinary Medicine
& Animal Sciences, University of Peradeniya
Technical support required For Sample Analysis
OBJECTIVES
To develop a sample strategy for milk & dairy products and to establish analytical capability for
stable isotopes and trace elements.
DESCRIPTION OF WORK
Task 1: Geographical mapping of dairy processing centers and the milk producers supplying to the same
processing plant within a range of 5km radius.
Task 2: Literature survey to find out methodology for extraction and analysis.
Task 3: Collect metrological data
Task 4: Establish liquid distillation procedures for processing milk samples
Task 5: Procurements
Task 6: Collect representative milk samples to derive baseline data
Task 7: Establish sampling milk & supplementary samples along with maintaining records
Task 8: Write and send an annual report to be evaluated by IAEA scientific board.
DELIVERABLES
No. Description Month
1 GPS maps for locating sampling sites December,2013 - April,2014
2 Literature Review will be available December,2013 - April,2014
3 Collect metrological data December,2013 – January,2014
4 Establish liquid distillation procedures for milk samples. December,2013 – August,2014
5 Availability of equipment and supplies January,2014 - August,2014
6 Collect representative milk samples August, 2014
7 Available milk samples at suitable storage conditions August, 2014
8 Progress reports will be sent through the institutes(AEA) September , 2014
EXPECTED RESULTS
Availability of sampling method & milk samples and supplementary samples in order to establish
baseline data