SAMPLING- process of removing an appropriate number of items from a population in order to make
inferences to the entire population SAMPLING PLAN- definite working rule regarding N (total
size/population), n (sample size) and c(# of defects)
SAMPLE- finite number of objects from a population
N(total size/population), n (sample size) and c(# of defects) :acceptance
number
✓ FINAL SAMPLE
Sample ready for the application of the test procedure.
✓ RANDOM SAMPLE
Sample in which the different fractions of the
material have an equal probability of being represented.
✓ SAMPLING PLAN
Description of the location, number of units
and/or quantity of material that should be collected, and associated
acceptance criteria.
✓ SAMPLING PROCEDURE
The complete sampling operations to be
performed on a defined material for a specific purpose. A detailed written description of the sampling procedure
is provided in the sampling protocol.
✓ 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.
✓ RETENTION SAMPLE
Sample collected as part of the original sampling process and reserved for future testing.
Representative of the batch of materials or products from which are they taken should be sufficient for at least 2
full re-examinations
✓ SAMPLER
Person responsible for performing the sampling
operations.
✓ SAMPLING METHOD
That part of the sampling procedure dealing
with the method prescribed for withdrawing samples.
✓ SAMPLE
A portion of a material collected according
to a defined sampling procedure. The size of any sample should be sufficient to allow all anticipated test procedures to
be carried out, including all repetitions and retention samples.
✓ SELECTED SAMPLE
Sample obtained according to a sampling
procedure designed to select a fraction of the material that is likely to have special properties.
✓ EXTREME SAMPLE
A selected sample that is likely to contain deteriorated, contaminated, adulterated or otherwise unacceptable
material.
✓ SAMPLING RECORD
Written record of the sampling operations
carried out on a particular material for a defined purpose. The sampling record should contain the batch number, date
and place of sampling, reference to the sampling protocol used, and a description of the containers and of the materials
sampled, notes on possible abnormalities, together with any other relevant observations, and the name and signature of
the inspector.
✓ SAMPLING UNIT
Discrete part of a consignment such as an
individual package, drum or container.
✓ PRODUCER'S RISK
risk of rejecting a good batch
✓ CONSUMER'S RISK
risk of accepting a bad batch
✓ 100% INSPECTION
o inspecting the entire batch/lot
o The cost of 100% inspection is PROHIBITIVE
o Labor intensive and the probability of rejecting the batch is HIGH
RANDOM SAMPLING
• In a random sample, all units/ parts have the same likelihood of being selected for inspection, whenever
possible each sampling unit should be consecutively numbered and the required number of random
sampling units selected using tables of random numbers.
SAMPLING PLANS FOR STARTING MATERIALS, PACKAGING MATERIALS AND FINISHED
PRODUCTS
For STARTING MATERIAL:
N-PLAN
• The n plan is based on the formula n = 1 + ÷N, where N is the number of sampling units in the consignment
• SQUARE ROOT SYSTEM
• Square root + 1
• Assuming a uniform material from a recognized
source where there is a high degree of confidence in the source
P-PLAN
• The “p plan” may be used when the material is uniform, is received from a recognized source and the main
purpose is to test for identity.
• The p plan is based on the formula p = 0.4 ÷N,
where N is the number of sampling units. The figures for p are obtained by rounding up to the next highest
integer.
• Assuming a uniform material from a recognized
source with the main purpose of checking the identity.
R-PLAN
• The “r plan” may be used when the material is suspected to be nonuniform and/or is received from a source that is not
well known.
• r plan may also be used for herbal medicinal
products used as starting materials. This plan is based on the formula r = 1.5÷N, where N is the number of sampling
units. The figures for r are obtained by rounding up to the next highest integer.
• Assuming the material is non-uniform and/or
from a source that is not well-known
For PACKAGING MATERIALS:
• The objective is to ensure that there is a low probability of accepting material that does not comply with the
predefined acceptance level.
• British Standard BS 6001-1, ISO 2859 or
ANSI/ASQCZ1.4-1993.
For FINISHED PRODUCTS:
• In some cases it may be sufficient to limit examination of finished goods to visual inspection only. If physical and
chemical testing is required, however, the sampling units should consist of whole packs. Individual packs should
not be broken open for the purposes of sampling.
• British Standard BS 6001-1, ISO 2859 or
ANSI/ASQCZ1.4-1993.
DIFFERENT TYPES OF SAMPLING PLANS FOR QC INSPECTION
CONTINUOUS (MIL-STD-1235B)
This approach makes sense when these conditions are met:
• Inspection is quick and results are known very
fast
• No destructive test is involved
• Product quality is known to be relatively stable
•
Products are identical (same materials going through the same process under the same specifications)
GOVERNMENT SAMPLING
PLAN/
MILITARY STANDARD
Military standard-A common sampling plan that uses master tables to interpret the results:
• AQL inspection
• MIL-STD-105D
o NORMAL
o REDUCED
o TIGHTENED
• ABC-STD-105D
• MIL-STD-414
“ACCEPTANCE ON ZERO”
This is common in industries such as automotive or pharmaceutical.
a. Incoming inspection - you need a cost-effective way of checking a number of batches.
b. In process control - the approach here is usually a combination of:
PROCESS CONTROL PRODUCT CONTROL
c. Final inspection
incoming - MIL-STD-105D
PURPOSE OF SAMPLING
• The tests to be applied to the sample may include:
o verifying the identity;
o performing complete pharmacopoeial or analogous testing; and
o performing special or specific tests.
Sampling facilities should be designed to:
• prevent contamination of the opened container, the materials and the operator;
• prevent cross-contamination by other
materials, products and the environment;
• protect the individual who samples (sampler) during the sampling procedure.
Responsibilities for sampling
Those responsible for sampling procedures include:
• governmental organizations, such as drug
control authorities (including inspectorates); quality control laboratories; customs
• customers such asuch as governmental or
nongovernmental agencies involved in the acquisition of drug products
• police authorities responsible for the clearance
of drug products held in quarantine after manufacture or importation, and for the detection of pharmaceutical
products that have deteriorated or have been contaminated, adulterated or counterfeited;
• manufacturers in the context of good manufacturing practices (GMP).
SAMPLING PROCESS
Preparation for sampling - sampling tools
All sampling tools and implements should be made of inert materials and kept scrupulously clean. After use or
before reuse, they should be thoroughly washed, rinsed with water or suitable solvent, and dried. They should be stored
in clean conditions.
The adequacy of the cleaning procedure for the material from which the sampling tool is made should be
demonstrated. The use of disposable sampling materials has distinct advantages.
SAMPLING OPERATION AND PRECAUTIONS
There should be a written procedure describing the sampling operation. This should include details of the health
and safety aspects of sampling.
STORAGE AND RETENTION
• The container used to store a sample should not interact with the sampled material nor allow contamination. It should
also protect the sample from light, air and moisture, as required by the storage directions for the pharmaceutical
product or related material sampled.
•
Security and adequate storage conditions should be ensured for the rooms in which samples are stored.
Samples should be stored in accordance with the storage conditions as specified for the respective active
pharmaceutical ingredient (API), excipient or drug product.