Title: Training Workshop on Laboratory Methods and Procedures for Persistent Organic Pollutants in Biological Tissues, 19-20 January 2009 : Summary report
Full Citation
Permanent Link: http://ufdc.ufl.edu/UF00095630/00001
 Material Information
Title: Training Workshop on Laboratory Methods and Procedures for Persistent Organic Pollutants in Biological Tissues, 19-20 January 2009 : Summary report
Physical Description: Book
Language: English
Creator: Caribbean Coastal Pollution Project
Publisher: UNU-INWEH
Place of Publication: Hamilton, Ontario, Canada
Publication Date: January 19-20, 2009
Copyright Date: 2009
 Record Information
Bibliographic ID: UF00095630
Volume ID: VID00001
Source Institution: University of Florida
Holding Location: University of Florida
Rights Management: All rights reserved by the source institution and holding location.


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Training Workshop on Laboratory Methods and Procedures
for Persistent Organic Pollutants in Biological Tissues
19-20 January 2009
Reef Yucatan Hotel, Merida Mexico

Caribbean Coastal Pollution Project (CCPP)
Assessment, Monitoring and Management of Persistent Organic Pollutants (POPs) and Persistent
Toxic Substances (PTS) in the Coastal Ecosystems of the Wider Caribbean Region

Summary Report



Prepared by: Hanneke Van Lavieren




Table of Contents

I. INTRODUCTION.................. .................................... ............ ................. .3

II. TRAINER AND PARTICPANTS..................................... ................................. 4

III. TRAINING COURSE ACTIVITIES............................................ .......................... 4

IV. PROCEEDINGS OF THE COURSE........................................... ........................... 5

V A N N E X E S ...................................... ..................................... ................ . 7


The Caribbean Coastal Pollution Project (CCPP) aims at the assessment, monitoring and
management of Persistent Organic Pollutants (POPs) and Persistent Toxic Substances (PTS) in
the Coastal Ecosystems of the Wider Caribbean Region (WCR) and commenced in September
2007. It is being funded by the World Bank through the Canada Persistent Organic Pollutants
Fund from the Canadian International Development Agency (CIDA) as well as by UNU-

The purpose of CCPP is to build a network among environmental managers, analytical
laboratories, and other appropriate governmental agencies in countries of the WCR that will be
key in measuring, evaluating and then reducing pollution from POPs and other PTS in coastal
marine environments. These reductions can be achieved through changes to behaviour that stem
releases of pollutants into the environment in upstream agriculture and industry.

Capacity Building

One of the aims of the project is to evaluate laboratory capacity by visiting existing lab facilities
and performing cross-calibration trials, implementing advanced training of laboratory personnel
through training workshops and secondments of staff to Canadian labs, and also providing for
instrumentation upgrades.

During May-June 2008, questionnaires were sent to all the participating laboratories to assess
their current capacity in terms of staff, infrastructure, laboratory equipment and capacity needs to
sample and analyze POPs and other PTS. The responses from these questionnaires were
synthesized by an expert team and used as preliminary information for an evaluation report. The
experts conducted ten laboratory visits during June-August 2008 and a Final Laboratory
Evaluation Report was submitted in October 2008.

Specific training needs were identified during the laboratory evaluation exercise and included
sample preparation and analysis, GC calibration, examples of different extraction and clean-up
methods, risk assessment, instrument detection limits and method quantization limits and quality
assurance and control. This training was the first training held in context of the CCPP. All
PowerPoint presentations can be found as PDF files at:
http://www.inweh.unu.edu/inweh/Coastal/POPs%20Monitoring/Merida/Presentations/1 Trainin
g.pdf or can be requested at: contact@inweh.unu.edu.

Objectives of the course

The objective of providing training is to build the understanding and capacity of laboratory staff
in our eight project countries in: 1) analytical and extraction methods for POPs in biological
tissues; and 2) methods and procedures for laboratory quality control/quality assurance

About the Trainers

Four trainers with extensive experience in environmental POPs issues conducted the training:

o Dr. Chris Metcalfe, Trent University
o Dr. Ken Drouillard, University of Windsor
o Dr. Gerardo Gold, CINVESTAV Unidad Merida, Mexico
o Ms. Nargis Ismail, University of Windsor

Selection of Participants

Invitees to the training workshops preferably have laboratory supervisory responsibilities and the
ability to pass along lessons learned to personnel under their supervision.


Training was held at the Reef Yucatan Hotel in Merida, Mexico, from 19-20 January 2009 and
the workshop programme is given in Annex 1 of this report. A total of 15 participants from the
eight project countries attended (the list of participants is given in Annex 2).

Course handouts

Course handouts comprised electronic versions of the presentations, as well as the following

Canadian Association for Laboratory Accreditation (Inc): T27 CALA 17025:2005
Handbook Revision 2.3 December 2007
GLIER Analytical laboratories Quality Manual
GLIER Quality System Procedures
Standard Operating Procedures GLIER Organic laboratory
Analytical methods for PCBs and organochlorine pesticides in environmental monitoring
and surveillance: a critical appraisal

These handouts are available at
or can be requested from contact@inweh.unu.edu.

During the morning of day 2 of training a practical laboratory exercise was organized at the
CINVESTAV laboratory, Unidad Merida campus, Merida. It gave participants an opportunity to
visit the laboratory and campus, and to see some hands on demonstrations of different extraction
techniques, and practice some of these techniques. It also gave them an opportunity to ask the

trainers specific questions and in exchange discuss different laboratory techniques used in their
own laboratories, discuss problems etc.


The final programme of the training workshop is given in Annex 1 of this report. The following
section provides a short summary of the workshop proceedings.

Day 1 19 January 2009

The participants registered at 8.30 am and the training was opened by Ms. Hanneke Van
Lavieren at 9 am.

Dr. Drouillard followed this with a session on Standard Operating Procedures for POPs and gave
an overview of the Analytical Methods for the Stockholm Convention Persistent Organic
Pollutants (POPs). It was mentioned that UNEP has no consensus SOP in place. Sample storage
and handling issues were discussed, as well as storage (temporary or long term) and sample
preparation. GC MSD and GC ECD methods were discussed including analyte extraction from
blood, milk- liquid and lipid contents: liver, muscle, adipose fin, and carcass. This session also
covered examples of different extraction and clean-up methods, the importance of clean up and
good instrument maintenance and instrument detectors and quality assurance.

This was followed by a session with Dr. Metcalfe on Chromatographic Techniques, Limits of
Detection and Calibration. Subjects covered included partitioning multiple partitioning of
multiple solutes, separation of analytes, elution Chromatography, stationary phase, clean ups,
size exclusion chromatography, analytical chromatography, and gas Chromatography.

Dr. Drouillard then conducted a session on Quality
Systems Documentation and its function and why it
is needed, elements of a Quality System Manual and
Accessory Documents and the GLIER QA Manual
Example. He discussed what is needed for
accreditation, audits, technical requirements,
Quality system Procedure, lab personnel, data
reporting and storing, lab equipment (QA and QC),
calibration, and lab monitoring guidelines.

Dr. Metcalfe followed with a session on instrument detection limits, and methods detection

After lunch, Nargis Ismail focused on How to validate your method. This covered approaches to
method validation, validation protocol, frequency of method validation, machine calibration,
performance parameters and troubleshooting.

Dr. Drouillard next presented Quality Control Charts and Evaluation of Data Integrity. This
included procedures for record keeping, Westgard Rules, the issuance of non-compliance reports,
control charts, database needs and validation, and database entry.

This day concluded with a short discussion session.

Day 2 20 January 2009

A practical laboratory and field day was organized from 9 am to 12 pm.

This included a laboratory demonstration and exercise on POPs extraction by cold column and
micro-methods, POPs cleanup by florisil and/or by silica as well as preparation and extraction of
a fish sample.

After lunch, Dr. Drouillard presented Data Reporting &Data
Management which included official data reporting, data
management, data back ups, data storage, QA Assessment and Sign-
off of data quality and data reports.

This was followed by Nargis Ismail who presented GC-Methods and
instrument maintenance. This included an overview of documented
Methods for POPs (OCs/PCBs) and basic maintenance and
troubleshooting, lab ware and sample collection, sample
homogenation before extraction, soxhlet extraction, column extraction, extraction scheme, GPC
columns, and bio beeds.

Dr. Drouillard then presented clean-up methods ofPOPs from Biological Samples, including
Gel Permeation Chromatography GPC Maintenance and Calibration Florisil Chromatography,
and Silica Chromatography.



Schedule for POPs Training Workshop for Laboratory Managers POPs in Biological

Day 1 Monday Jan 19

9:00 9:45 am

9:45 10:15 am

10:15 10:30 am

10:30- 10:45 am

10:45- 11:30 am

11:30-12:00 pm

12:00 1:00 pm

1:00 2:00 pm

2:00 2:45 pm

2:45 3:00 pm

3:00- 4:30 pm

Overview of SOPs for POPs in tissues (GC-ECD) (Drouillard)
-Examples of different extraction and clean-up methods
e.g. EPA and other accredited methods are reviewed

Introduction to chromatographic techniques (Metcalfe)

The Quality Assurance Manual (Drouillard)
-Components of a QA manual
-GLIER manual as an example


-Instrument Detection Limits and Method Quantitation Limits (Metcalfe)
-Overview of approaches to determining instrument detection and method
quantitation limits with specific reference to gas chromatography and POPs

How to Validate Your Method (Ismail)
-Approaches to method validation, Frequency and Troubleshooting

Quality Control Charts and Evaluation of Data Integrity (Drouillard)
-Record keeping, Westgard Rules, Issuing Non-compliance reports


POPs extraction methods (Ismail/Gold/Metcalfe)
-Cold Column, Micro-Cold Column, Sonication, Soxhlet, ASE, Other
-Where available overview of literature comparisons across methods
-Note for Satellite labs attention must be placed on infrastructure needs (e.g.
ventilation, solvent cabinets etc.), equipment, supplies
-Appropriate spiking internal standards, blanks, CRMs etc.


-Clean-up of POPs from Biological Samples (Drouillard)
-Florisil/Alumina/Silica Gel/GPC

4:30 5:00 pm Discussion

Day 2 Tuesday Jan 20

9:00 9:30 am Tour of CINVESTAV Laboratory

9:30 10:30 am Laboratory Exercise (Ismail/Gold)
-POPs extraction by cold column and micro- methods
-Extraction of CRMs according to SOP (3 stations?)

10:30 10:45 am BREAK

10:45 12:00 pm Laboratory Exercise (Ismail/Gold)
-POPs cleanup by florisil and/or by silica

1:00 2:45 pm Lunch and Return to Conference Room

2:45 3:30 pm GC-Methods and instrument maintenance (Ismail)
-Documented methods for POPs (OC/PCBs)
-Basic maintenance and trouble shooting

2:45 3:30 pm Data base management/QA Summary/Data Report (Drouillard)
-Data storage and back-ups
-The QA Assessment and Sign-off of data quality
-The Data Report

3:30 3.45 pm Break

3.45 4.45 pm GC calibration techniques (Metcalfe)

4.45 5.30 pm General discussion and evaluation of training.


Participants List

I isaias Maji1 tisnenes Department, Mimstry o0 Agnculture, r snenes & isaias.majl(a gmail.com
P.O. Box 148, Princess Margaret Drive
Belize City, Belize
Tel: 501-223 2623 ext. 24

2 Ramon Antonio Lab. Ciencias Nucleares ramondelanoy@yahoo.com
Delanoy de la Instituto de Fisica
Cruz Universidad Autonoma de Santo Domingo
Santo Domingo, Republica Dominicana
Tel: 1 809 689-7184
Cell: 1 809 330-2709
3 Juan Jos6 Arias Director jjariasd@yahoo.com
Dipr6 Instituto de Quimica de la Universidad Aut6noma de Santo
Domingo (UASD)

4 Dr. Bessie Oliva Universidad de San Carlos de Guatemala bessieoliva@yahoo.com;
Departamento de Analisis Inorganico, Laboratorio de bessie2@ intelnett.com
Edificio T-12 Segundo Nivel
Ciudad Universitaria Zona 12
Tel: (502) 52026232; 22887808
Fax: (502) 24767728
5 Marta del Cid Quality Manager mm.dc.m@0hotmail.com
Departamento de Analisis Inorganico, Laboratorio de
Facultad de CCQQ y Farmacia de la Universidad de San
Carlos de Guatemala

6 Indira Katania Head, Chemical Pollutants Unit jkatania"'y ahoo corn
Sierra Centro de Estudios y Control de Contaminantes

7 Raymond Reid Senior Analyst rrreidl@yahoo.com;
Department of Chemistry raymond.reid uwimona.ed
University of the West Indies u.jm
Mona, Kingston 7, Jamaica
Tel: 876-927-1910; 876-512-3116
Cell: 876-426-6978
Fax/Phone: 876-970-3878
Fax: 876-977-1835; 976-970-3878

8 Sherine Whyte Analyist, Department of Chemistry smarwhyte@yahoo.com
University of the West Indies
Mona, Kingston 7, Jamaica
Tel: 876-927-1910; 876-512-3116
Cell: 876-426-6978
Fax/Phone: 876-970-3878
Fax: 876-977-1835; 976-970-3878

9 Ing. Adriana Ing.Resp. Lab. Institucional de Quimica azavala@ecosur-qroo.mx
Zavala ECOSUR-Unidad Chetumal
Av. Centenario Km. 5.5 C.P. 77014
Chetumal, Quintana Roo
Tel. 01 983 83 5 04 40 ext. 4800
Fax 01 983 83 5 04 54

10 Ma. Guadalupe Quality Manager gnieto ecosur.mx
Nieto L6pez ECOSUR
11 Victor Ceja Lab Manager vceja @mda.cinvestav.mx

12 Mrs. Allison Laboratory Manager, CEHI aastwood@cehi.org.lc;
Astwood Caribbean Environmental Health Institute astwoodcehi@yahoo.com
P.O. Box 1111, Castries, St. Lucia
Tel: 758-452-1412/2501
Fax: 758-453-2721

13 Ms. Wendy Research Officer/Chemist wnorville@ima.gov.tt
Norville Institute of Marine Affairs
Hilltop Lane, Chaguaramas
Trinidad and Tobago, W.I.
Tel: (868) 634-4291 Ext.307
Fax: (868) 634-4433

14 Dr. Darryl Officer in Charge, Marine Chemistry Department dbanjoo@ima.gov.tt;
Banjoo Senior Research Officer Chemist, Institute of Marine Affairs banjoodarryl hotmail.com
Hilltop Lane, Chaguaramas
Trinidad and Tobago, W.I.
Tel: (868) 634-4291 Ext.309
Fax: (868) 634-4433

15 Dr. Denise Lecturer dbeckles @fsa.uwi.tt
Beckles Department of Chemistry
Faculty of Sciences and Agriculture
University of the West Indies
St. Augustine, Trinidad and Tobago, W.I.

16 Gerardo Gold Departamento de Recursos de mar, CINVESTAV Unidad ggold mda.cinvestav.mx
Bouchot Merida, Km 6 Antigua Carretera a Progreso Merida, Yucatan
97310 Mexico
Tel: +52 (999) 981 2927

17 Ken Drouillard Head Organic Analytical Laboratory kgd@uwindsor.ca
Associate Professor Biological Sciences
Great Lakes Institute for Environmental Research
University of Windsor
401 Sunset Ave.
Windsor, ON, N9B 3P4, Canada
Tel: (519) 253-3000 ext. 4744
Fax: (519) 971-3616

18 Nargis Ismail Lab Coordinator nargisi@,uwindsor.ca
Great Lakes Institute for Environmental Research (GLIER)
University of Windsor
401 Sunset Ave., Windsor
Ontario, Canada N9B 3P4
Phone: (519)253-3000 ext. 3450
Fax: (519) 971-3616

19 Chris Metcalfe Professor, Environmental & Resource Studies Program, Trent cmetcalfe@trentu.ca
Director, Watershed Sciences Centre
1600 West Bank Drive
Peterborough, Ontario, K9J 7B8
Tel: (705) 748-1011 ext. 7272
Fax: 705-748 1569

20 Hanneke Van UNU-INWEH vanlav@inweh.unu.edu
Lavieren 175 Longwood Rd S
Suite 204
Hamilton ON, L8P OA1



The Most Useful Parts of the Course:

Through the review of the evaluation questionnaires, it was apparent that most found the laboratory
visit with hands on exercises and the lectures and guidelines that dealt with practical aspects of sample
preparation and analysis the most useful parts of the course. Respondents also highlighted that the
presentations on control charts, westgard rules and detection limits were useful. Some found the
session on spiking internal standards, and elution of sample extract for PCB and organochlorine most
useful and the session on quality system documentation manual and procedures was also found to be
useful by a few respondents.

Moreover, respondents highlighted that during the workshop they were able to network, exchange
information and discuss issues amongst each other which was found useful.

The Least Useful Parts of the Course:

Most respondents said that the entire course was useful. It was felt by some that there was some
duplication and others found that sessions were too short and did not go into enough depth of the
subjects. Some suggested the use of practical exercises to apply the new techniques that were

A few mentioned that the accreditation requirements and data reporting sessions were not so useful
mostly because this is not part of the work of the respondents.

Difficulties in Applying:

Regarding the application of this workshop, there was some variance in response most mentioned
however that they would have no difficulties in applying what learnt. Some indicated they would have
some difficulty in applying validation and calibration techniques.

The Overall Feelings about the Course:

It was stated by almost all of the participants that their overall feeling about the course was well
programmed, well prepared, useful, and very productive. It was mentioned that it was useful to discuss
the different perspectives and examples from the countries amongst themselves and share knowledge
and discuss experiences and needs.

A few participants mentioned the need for more hands on exercises and longer visit to the laboratory.
Some indicated the sessions and overall course was too short. Most were happy to attend the course,
learnt a lot and looked forward to applying it in their work.

Other Comments:

In addition to the above comments, the need for more exercises after each session would have been
useful. Some mentioned that a few of the power points used too small fonts. Most indicated they would
need more practical lab training.

Summary Chart of Feedback in Section 2 of Evaluation Questionnaire

Suggestions for training workshops on related issues:



6--- -- --- -- -- ---- -- ---

4 -- --- -- --- -- -

2 -- g ood

I I | | excellent

* Data interpretation

* Hands on laboratory training in sample preparation and analysis procedures

* Distribution of POPs

* Use of biological markers e.g. Oysters

* Sample extraction, GC methods

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