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Interregional Seminar for Quality Control Laboratories involved in WHO Prequalification Programme and/or participating in respective sampling
and testing projects, Nairobi, Kenya, 23-25 September 2009
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Before sampling
I.
purpose of sampling?
II.
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Sampling process
I. Preparation for sampling
II. Sampling operation
III. Sample storage and retention
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Sampling tools should be available to the sampler, e.g. to open containers (knives,
hammers,...), material to reclose the packages (sealing tape), self-adhesive labels to
indicate that some of the contents have been removed, etc...
Sampling tools should be made of inert materials (e.g. polypropylene or stainless steel;
avoid glass) and kept very clean. After use, thoroughly washed, rinsed with water or
suitable solvent, dried and stored in clean conditions.
Washing facilities should be located in, or close to, the sampling area.
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Spatulas
for solids
Dip tubes
for liquids
Sample thieves
for solid samples in
deep containers
Bag-sampling
spears for taking
samples from bags
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
II - Sampling operation
Sampling plan: description of the location, number of units and/or quantity of material that
should be collected, and associated acceptance criteria.
Make sure that representative samples are taken in sufficient quantity. Representative
sample: sample obtained according to a sampling procedure designed to ensure that the
different parts of a batch or the different properties of a non-uniform material are
proportionately represented.
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Sampling operations should be supervised and documented => sample collection form
=> always kept together with the collected sample.
Sample collection form: written record of the sampling operations, containing: batch
number, sampling date/place, reference to sampling protocol used, description of
containers and materials sampled, possible abnormalities, any relevant observations,
name/signature of the sampler...
Store the sample in a properly labelled container: sample type, name of material,
identification code, batch number, code, quantity, date of sampling, storage conditions,
handling precautions, container number....
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Page 1
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Page 2
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Take into account previous experience with the product and supplier.
Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Containers used to store a sample should comply with the storage directions for
the active pharmaceutical ingredient, excipient or drug product:
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Security and adequate storage conditions (light, ventilation, safety requirements, and
any special requirements) should be ensured for the rooms in which samples are
stored.
Samples should be stored according to the storage conditions as specified for the
respective API, excipient or drug product.
Packaging materials similar to those in which the bulk is supplied should be used for
long-term storage.
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Screw-top containers
II. Inspections
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
The extent of the routine surveillance programmes for drug quality, carried out by
National Drug Regulatory Authorities will depend on:
The programme should include marketed products, whether registered for sale or
prepared in pharmacies.
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
The responsible laboratory should prepare the sampling programme (if needed
under the guidance of the drug regulatory authority) every year or half a year.
Sampling programme:
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
II - Inspections
Inspectors may take samples from:
retail or hospital pharmacies (including preparations manufactured in bulk in
the premises)
industry
wholesalers
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Starting materials
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
http://www.who.int/medicines/areas/quality_safety/regulation_legislation/certification/en/
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Sampling and testing may be adjusted according to the experience with the
source of the product, e.g. manufacturer or supplier.
*Consignment: quantity of a bulk starting material or drug product, made by one manufacturer or supplied by
one agent, supplied at one time in response to a particular request (1 or more containers, 1 or more batches).
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Sampling plans
I. Starting materials
II. Finished products
III. Packaging materials
Note: guideline primarily addressed to Drug Regulatory Authorities, these
sampling plans might not be appropriate for manufacturers.
The following plans are examples
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
II. p-plan
III. r-plan
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
I The n-plan
Only used when material is considered uniform and from a recognised source.
n 1 N
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
NOTES:
The n-plan is NOT statistically based and should be used only as a guiding
principle.
The n-plan is NOT recommended for use by control laboratories of
manufacturers that are required to analyse and release or reject each
received consignment of the starting materials used to produce a drug
product.
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
II The p-plan
May be used when material is considered uniform, from a recognised source and
the main purpose is to test for identity.
p 0 .4 N
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
May be used when material is considered non-uniform and/or obtained from a not
well know source.
r 1.5 N
Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
ISO 2859-2:1985 - Part 2: Sampling plans indexed by limiting quality (LQ) for isolated
lot inspection
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Practical example
http://www.ages.at
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
4
5
6
10
11
9: batch number
10: quantity
11: unit
12
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Step 4: Sampling
request sent by fax
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
4: expiry date
2
3
4
5: MA-number
5
6
6: manufacturing date
7: place of withdrawal (company,
wholesaler, pharmacy, others)
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
Part 2
2: light protection
2
3
3: temperature
5: prohibition of sale
6
6: crosscheck
7: sealing executed
8
8: certificate of analysis
9: composition/formulation
10: date of withdrawal/signature
10
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
2
3
4
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
References
WHO guidelines for sampling of pharmaceutical products and related materials. Annex 4 of
WHO Technical Report Series No. 929 (2005).
ISO 10725:2000 - Acceptance sampling plans and procedures for the inspection of bulk materials.
Good Manufacturing Practices; Part I - Basic Requirements for Medicinal Products ; Part II - Basic
Requirements for Active Substances used as Starting Materials.
European Pharmacopoeia. Chapter 2.8.20. Herbal drugs: sampling and sample preparation.
ANSI/ASQ Z1.4-2008 Standard (American National Standards Institute/American Society for Quality)
- Sampling Procedures and Tables for Inspection by Attributes.
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009
http://www.edqm.eu
Thank you for your attention
Marta Miquel
Scientific Officer
Council of Europe
European Directorate for the Quality of Medicines and HealthCare (EDQM)
Biological Standardisation, OMCL Network & HealthCare Department (DBO)
7 Alle Kastner, CS 30026
F- 67081 Strasbourg, France
Tel.: + 33 (0) 3 90 21 42 41
Fax: + 33 (0) 3 88 41 27 71
E-mail: marta.miquel@edqm.eu
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Sampling and testing for Quality Control Laboratories, Nairobi, September 2009