A defined master template of a document
ensures uniformity in knowledge management and compliance. Importance of
capturing correct information during development studies can never be
overemphasized.
Component of Method Qualification/Validation
protocol are listed below to ensure consistency in document format and
information capturing during the study. A protocol shall:
·
be identified with a number and date,
·
study title
·
contain name and titles of the investigators
and personnel supervising the study along with address,
·
contains names and titles of authorized
personnel who approve the study design,
·
protocol effective date.
The
contents of protocol shall include (but not limited to) the following:
1
OBJECTIVE
(Specific objectives providing statement of research
question(s) shall be provided under this section. The objectives shall be
stated in advance and shall not be depended upon research outcome. Like other
objectives, the objectives of qualification/validation study shall be SMART (Specific, Measurable, Achievable,
Relevant and Time Bound). After statement of the primary objective,
secondary objectives may be mentioned.).
2
SCOPE
(Scope is defined as the extent of the area or subject
matter that something deals with or to which it is relevant. The scope of protocol shall indicate "when" the study needs to be performed and "where" it applies.)
3
INTENDED USE OF METHOD
(This section shall define "why" the protocol is being written,
study designed and where the final method will be used. Based on objective and
scope, details of intended use of method with respect to samples (at different
stages of process) shall be provided.).
4
RESPONSIBILITY
(Provide details of “who” performs
the procedure and who is responsible to see it is performed correctly. Responsibilities
for each critical stage such as sample provisions, sample storage, preparations
of reagents and solutions, testing, data recording, data review, data archival,
study approvals etc., shall be provided. Tabulated representation is preferred).
5
DEFINITIONS & ABBREVIATIONS
(Provide definitions with respect to
study and internal systems with will clarify the strategy and study plan. List
of abbreviations used shall be provided).
6
SAFETY CONSIDERATIONS
(Provide safety considerations and
precautions for work with respect to physical, instruments, equipment, chemicals,
bio-hazard, sample, reagents/solutions, disposal and spill control with
available person safety tool requirements etc.)
7
INTRODUCTION
(This is where the protocol differs
from SOP. An introduction shall provide background of test method/equipment and
instrument principle, source of selected test method, application and scope of
the test method, rationale for selecting the test method for specified sample analysis.
Relevant references shall be provided).
8
MATERIALS
(This section along with section 9,
10, 11 & 12 defines “what” is needed to perform the test. The list should
be complete and specific Details of material used in study with respect to
material description, make, catalogue number/part number, quantity. This should
include chemicals, reagents, consumables, etc. Tabulated representation is
preferred).
9
EQUIPMENT AND INSTRUMENTS
(Details of equipment’s and
instruments used in the study with make, model, ID No, Reference SOP,
calibration and qualification requirements etc. shall be provided under this
section).
10
REAGENTS AND SOLUTIONS
(Details of reagents and solutions to
be used in study shall be provided. Ready to use solutions and reagents shall
be listed first with details such as solutions/reagent description, make,
catalogue number/part number and storage details in any. Subsequently the
description of reagents and solution to be prepared shall be provided with
standard formulae and step wise preparation procedure followed by storage
conditions and use before date. It is preferable to identify the critical
reagents used in the study).
11
SAMPLE DETAILS
(Details of sample with respect to
sample description, sample source, process stage, matrix details, storage
conditions, handling instructions if any shall be provided. Wherever sample
preparation is required before analysis, relevant details shall be provided.)
12
STANDARD DETAILS
(Details of standard with respect to
standard description, sample source/make, catalogue number, matrix details,
storage conditions, handling instructions if any shall be provided. Wherever
standard preparation is required before analysis, relevant details shall be provided.)
13
METHOD DESCRIPTION/ METHOD REFERENCE
(Clear concise, step by step
instructions on "how" to perform the test. This should be written as instructions
for the operator to follow, without a lot of theoretical background. A section
on fundamental principles can be included if necessary. Wherever, applicable a
method reference shall suffice.).
14
STUDY PLAN/ DESIGN/PARAMETERS TO BE STUDIED
Clear concise, step by step
instructions on how study will be performed. Provide details of each parameter
to be studied, with justification/selection criteria.
Each parameter shall be elaborated in
following sub headings:
·
Parameter
Name/Description:
·
Test
Procedure
·
Calculations
and Statistical analysis
·
Acceptance
Criteria
·
Documentation
(record of data during analysis)
Following parameters are usually
studied during method qualification / validation (depend upon the strategy
adopted):
·
Specificity
·
Linearity
and Range
·
Precision
o Method precision (Repeatability)
o Intermediate precision (Ruggedness)
·
Accuracy
·
Limit
of Detection (LOD)
·
Limit
of Quantification (LOQ)
·
Robustness
·
Solution/Reagent
stability
·
Forced
Degradation study
·
System
Suitability
15
STUDY PLAN SUMMARY
Summary of Study Plan with samples,
number of replicates, number of repeats and, day of analysis shall be provided,
preferably in tabulated form.
Replicates and repeats are
distinguished as below:
Replicates (Measurement Replicates): These
are repeated measurement of same item, i.e., single sample is measured more
than once in same experimental run.
Repeats: Here implies to repeated experiment from sample preparation to measurement, an independently repeated data.
Wherever, data from one parameter is
used in analysis of the other parameter, details of such strategy shall be
provided.
16
DOCUMENTATION AND DATA RECORDING
This section details “What Next”
a) Indicate where the results should
be recorded.
b) Explain what to do if there are
problems during the test.
c) Indicate that deviations to the
procedure must be approved and recorded.
d) Identify the person to whom the
final results should be reported.
Details of documentation and data
recording strategy adopted to ensure complete, consistent, accurate data which
shall be contemporaneously recorded).
17
REVALIDATION/REQUALIFICATION CRITERIA
(Wherever applicable,
revalidation/qualification criteria shall be mentioned).
18
REFERENCES
(List of references consulted during
the experimental studies)
19
ENCLOSURES
(Provide list of enclosures to protocol, this may include
flow charts, tabulated strategy with acceptance criteria etc.)
Wherever contemporaneous record of the experiments need to
recorded, a record forms shall be annexed with the Protocol.)
20
HISTORY
(Provide details of document history
in below table).
