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Philippine Institute of Pure and Applied Chemistry

GLP Characterization:
Test Items and Test Systems
Giselle Grace Lim- Co Yu Kang
Department of Chemistry
Ateneo de Manila University

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“To perform good

scientific studies, it is
best to know as much
as possible about the
materials used in the
experiments.”
Good Laboratory Practice Training Manual 2nd ed.
World Health Organization, 2008

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GLP Characterization involves:

• Test Item
• Test System

Test Test Test

item System Result

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TEST ITEM
 Any article that is the subject of the study

What are test items?

 Active ingredient for medicine
 Pesticide
 Food additive
 Industrial chemical compound
 Plant extract

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TEST ITEM A catalyst for progress

 Characterized by its analytical profile

 Chemical identity
 Impurity
 stability
To prevent false results, it is important that test items
are protected from cross contamination.
GLP principles require that proper conditions for
receipt, handling and storage of the test items are in
place.
What are the factors that could compromise the test
item?
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A. Chain of Custody

Sampling
Labs must comply with
strict instructions
Receiving of
Samples  Failure to do so
jeopardizes the results
Endorsement
to Analyst
 Must be well-
Disposal/ Return to documented
Client

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Sampling
 Sampling
Based on appropriate statistical methods
 Record all relevant data and operations
Manufacturer’s name, date of sampling,
types/ quantities of contents, identity, batch
number, person who conducted the
sampling, name of transporter and type of
Endorsement
carrier
to Analyst
 Maintain the integrity of the sample
• Strong enough to withstand transport
• Types of containers (glass, plastic, etc.)
• Temperature of transport (frozen, cooled)
• Factor in unexpected situations (traffic,
brownout)
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Sampling
 Sampling
Practice proper identification of samples
 Must be unique, not used cyclically
 System
Receiving ofof naming must be unambiguous
 Sample code must be written in all reports
Samples
(traceability)

Give an example of an appropriate sample ID which

complies to the characteristics mentioned above.

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Receiving of Samples
 Staff must be informed in advance when the test
Sampling
item will arrive to ensure proper storage conditions
and necessary handling requirements
Receiving of
 Staff logs the arrival and identity of samples as soon
Samples
as possible to demonstrate that test items were not
held in conditions that will compromise its chemical
activity
 Specific instructions on sample receiving must be
available (if designated staff is absent)
Disposal/ Return to
 Information on the test item must be cross-checked,
Client
records of each delivery is kept, any discrepancies
should be noted
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Storage
 Procedures
Sampling and facilities to avoid sample
deterioration and contamination must be in place
 Storage conditions must be maintained, monitored,
and recorded
 Controlled access to storage
 Items can be signed in and out in a logbook

Disposal/ Return to
Client

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After the analysis
1. Retained Sample
Sampling
 Important especially when results have to be
reviewed, re-tested
 Clear policy on how long samples will be kept
2. Return to Client
 Ensure that items are properly packed and
transported to maintain integrity of the results
3. Waste Disposal
Disposal/ Return to
 Provision
Client for appropriate collection, storage, and
disposal facilities; decontamination and disposal
procedures
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Exercise: Provide a risk that may happen if GLP was not
practiced in each step.

Sampling

Receiving of
Samples

Endorsement
to Analyst

Disposal/ Return to
Client

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B. Raw materials/ Reagents
 Labelled properly (include concentration) for
identification
 Preparation/ expiry date
 Storage instructions
 Source
 Stability
 Waste disposal

Name of Reagent :
Date Prepared:
Expiry Date:
Prepared by:
Waste Code:

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Reference Standards
 provides a basis for comparison with the test
analyte
 calibrated by a body that can provide the required
traceability
 Used for calibration only
 Must be traceable to the International System of Units
(SI).
 Transport and storage must be ensured to protect its
integrity. Store away from test items to prevent
contamination; must not be placed in the same
location as samples

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Key Questions for Self-Assessment A catalyst for progress

Do you have procedure for logging samples and

other items into the laboratory?
Are samples, standards, and reagents uniquely
numbered upon receipt?
Do you follow a system wherein the items are stored
securely and preserved against changes that might
affect the results?
Can you ensure that all procedures regarding
reagents are clearly communicated to all personnel?
Do you have a procedure to ensure reports are
checked to make sure they correspond to raw data?
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TEST SYSTEM
 Any biological, chemical, or physical system, or a
combination thereof, used in a study
What are test systems?
 Test animals
 Plants, bacteria, organs, cells
 Analytical equipment
Conditions and processes must satisfy the scientific
requirements of the study.
GLP requires an explanation in the protocol why a
particular test system has been chosen for a particular
study.
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A. Biological Test Systems (Test Animals)

Establish proper conditions for storage, housing, handling,

and care; Isolate until health status has been evaluated

Maintain records of source, arrival date and conditions;

Acclimatise to the test environment prior to the first
application of the test item

Indicate all needed information on the housing or containers

Routinely clean and sanitize the housing or containers
during use. Use of pest control must be documented.

In field studies, location must be free from

interferences (spray drift, pesticides)
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B. Analytical Equipment
Equipment Records
 complete history of the equipment, detailed
record of all calibrations, repairs, maintenance
and performance checks.
 Must be within the proximity of the equipment
 Each equipment must be issued a unique
identifier, especially if several units of the same
type are in use.

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B. Analytical Equipment
Commissioning of New Equipment
 Checks against the manufacturer’s specification
and checks to confirm that the equipment gives
satisfactory results for the measurements it is
intended
 Calibration before use
 Properly label equipment under trial so as not
to be used for routine work

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B. Analytical Equipment
Service/ Calibration Schedule
 Both from the supplier and in-house
 Most equipment requires formal checks even if
it is effectively checked with the standards at
each use
Equipment Log
 Usage logbook
 Every action taken (service, trouble shooting,
routine checks, etc.) must be recorded
 Service reports, calibration certificates, output
from performance check should also be attached.
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B. Analytical Equipment
Equipment Labeling and Sealing
 Each piece of equipment should carry a label
indicating last calibration date and date when
next due.
 Staff should be properly instructed that
equipment that are overdue for check or
calibration are not to be used.

Regular/ preventive maintenance

 QA checks

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Key Questions for Self-Assessment A catalyst for progress

Do you have a system for commissioning equipment

and verifying its performance and calibration
before it is used for test?
Do you have a plan for periodic calibration and
verification of the performance of all equipment
which affects validity of measurements?
Do you have records showing that this plan is
followed and which enable the status of any
equipment to be verified at any point in its history of
use?
Is equipment subject to regular checks or
calibrations labelled so that its status can be seen
immediately by users?
22
Complying with ISO 17025; Philippine Institute
A practical guidebook for of Purethe
meeting and Applied Chemistry
requirements of laboratory accreditation schemes based on
ISO 17025:2005 or equivalent national standards, 2009, United Nations Industrial Development Organization.
 In partnership with industry,
A catalyst for progress
Discussion Questions:

1. What are some “malpractices” or points for improvement

that we have observed in our individual workplaces (in the
context of instrument usage or in keeping reagents/
standards)?

2. What are some corrective or proactive actions that we

commit to do at work after this seminar?

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C. Analytical Methods

 Standard methods
 In-house methods based on standard specifications
 In-house methods

 Must be relevant to the company’s or the client’s

needs
 Lab must show that it can deliver
consistent data within known limits

 Lab must test itself against agreed

reference points
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Standard Methods
• Sampling
Published in literature
1. ISO standards
2. American Society for Testing and Materials
(ASTM)
3. AOAC Methods
4. USP

• Full method validation is not required, but needs

verificationReturn to
Disposal/
• The ability to achieve the performance required of the
Client
standard specification must be shown

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In-House Methods Based on
Standard Specifications
Sampling
• Modified version of the standard method
• Reduced amount of validation needed (depending on
the degree of deviation from standard method)

In-House Methods
• Laboratory-developed
• Method validation is necessary
• Must be technically sound and suitable for the
purpose claimed
• Effective communication among personnel involved is
important
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identification
Uncertainties Scope

Data, method Description of

of analysis test item
In-House
Criteria of Methods Parameters;
acceptable data Quantities range

Technical
Procedure
requirements

Environmental Reference
conditions materials 27
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Method Validation
• Confirmation that the analytical method is fit for
purpose

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Method Validation
• Values obtainable from validated reports:
1. Scope of applicability
2. Uncertainty of the results
3. Detection limit
4. Selectivity of the method
5. Linearity
6. Limit of repeatability/ reproducibility
7. Robustness
8. Cross-sensitivity

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Interlaboratory proficiency testing

 Effective extension to the internal quality control

procedures
 Traceability when certified reference materials
are not available

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Key Questions for Self-Assessment A catalyst for progress

Do you have a set of acceptable methods?

Are they documented well enough to be applied

properly and consistently?
What is the accuracy, precision, and the limit of
detection of the methods/equipment used?

Do you run routine quality control (QC) samples and

evaluate the results prior to releasing data?

Do you monitor trends in QC results and use these

to foresee possible problems?
Have you tested your methods through certified
reference methods and/or interlab comparison?
31
Complying with ISO 17025; Philippine Institute
A practical guidebook for of Purethe
meeting and Applied Chemistry
requirements of laboratory accreditation schemes based on
ISO 17025:2005 or equivalent national standards, 2009, United Nations Industrial Development Organization.
 In partnership with industry,

References A catalyst for progress

Complying with ISO 17025; A practical guidebook for meeting the

requirements of laboratory accreditation schemes based on ISO
17025:2005 or equivalent national standards, 2009, United Nations
Industrial Development Organization.

OECD Principles on Good Laboratory Practice (as revised in 1997), 1998,

Organisation for Economic Co-operation and Development.

Good laboratory practice training manual for the trainer: a tool for training
and promoting good laboratory practice (GLP) concepts in disease
endemic countries - 2nd ed.World Health Organization, 2008

ISO/ IEC 17025: 2005; General requirements for the competence of testing
and calibration laboratories.

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