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4.
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PROCEDURE
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4.1.
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Analytical Method Transfer Protocol (AMTP)
and Analytical Method Transfer Datasheet cum Report (AMTDR) shall be prepared
after completion of method validation and approved Standard Test Procedure
(STP).
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4.2.
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Data generation for technology transfer
shall be initiated after approval of Analytical Method Transfer Protocol.
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4.3.
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Blank Analytical Method Transfer Datasheet cum Report shall be
approved along with protocol and same shall be made effective prior to
execution of technology transfer activity.
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4.4.
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Data shall be reported subsequently after
analysis of both units i.e. (Transfer Unit and Receiving Unit) in Analytical
Method Transfer Datasheet cum Report.
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4.5.
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If validation is carried out in-house then
method precision or intermediate precision data shall be taken for analytical
method transfer activity.
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4.6.
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If the formulation is proportionally
similar (dose weight) then the technology transfer shall be performed on
higher strength only.
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4.7.
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If the formulation is not proportionally
similar (Pseudo dose) and the product has multiple strengths, then the
technology transfer shall be performed on lowest and highest strengths.
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4.8.
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If the formulation has multiple groups of
proportionally similar formula, then the technology transfer shall be
performed on highest strength of each group.
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(For e.g. 0.25 & 0.5 mg strengths are dose
weight proportionate, 2,3 & 4 mg are dose weight proportionate and 1 mg
are dose weight proportionate, then validation shall be carried out on 0.5, 4
and 1 mg strength)
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4.9.
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If validations perform outside laboratory
such as Contract Research Organization (CRO) in that situation transfer of
analytical method shall be perform by CRO to Quality Control of Ajanta Pharma
(Receiving Unit). The transfer of analytical method(s) can be done by
Collaborative study.
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4.10.
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The transfer of analytical method(s) can be
done by methods as
a) Collaborative study
i) Indirect Method
transfer
ii) Direct Method
transfer
b) Co-validation between two or more
laboratories
c) Revalidation
d) Transfer Waiver
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4.10.1.
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Indirect Method Transfer:
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4.10.1.1.
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An approach to transfer analytical method(s)
that involves analysis of common samples at two different laboratories using
the same analytical method.
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Sr. No.
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Actions
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Responsibility
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1.
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Initiate the analytical
method transfer.
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ADL in consultation
with QC
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2.
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Issue current Standard
Test Procedures to QC. Analytical method transfer is to be done using the
current specifications and STPs.
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Documentation, Research
Centre (TU)
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3.
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Prepare Analytical
method transfer protocol and Datasheet cum report & after assign a
protocol number to it.
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ADL and QA (TU)
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4.
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Checking, reviewing and approving the Protocol
and Datasheet cum Report
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ADL, QA (TU) and QC, QA (RU)
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5.
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Share any specific and
critical information regarding the method of analysis with the QC.
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ADL
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6.
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Send the sample of same
batch / lot along with the working standard(s) to the QC.
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ADL
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7.
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Test the samples in both Laboratories using the
same working standard(s) and using the same standard testing procedure as
per the protocol. The time duration between the two analyses in both
locations is not more than two months.
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ADL and QC
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8.
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In case of time duration more than two months
or analytical method validation carried out at outside party; analyze the
sample at both the locations.
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ADL and QC
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9.
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Certification shall be done after completion of
Technology Transfer.
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QC, QA(RU), QA (TU) and Head (RC)
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4.10.1.2.
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If the acceptance criteria do not meet in case of collaborative study,
Head of QC shall analyze the data to look for any ambiguity. The method can
then be transferred with proper justification given for that. If failure
still persists, QC shall perform tests again. Sample conditions should also
be evaluated to check possible degradations. Failure shall lead to Direct
Transfer.
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4.10.1.3.
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For failure, where analysis involves only Direct Transfer, the
analysis shall be repeated using the same batch.
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4.10.1.4.
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If the method does not meet the acceptance criteria even after the
repeat analysis, the follow up action shall be decided by Head of QC.
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4.10.2.
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Direct Method Transfer:
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4.10.2.1.
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An approach to transfer the analytical
methods in which the scientist from the Analytical Development Laboratory
demonstrates the method to the analyst of the Quality Control Laboratory.
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Sr. No.
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Actions
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Responsibility
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Perform method transfer at the QC.
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ADL and QC
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Prepare Analytical method transfer protocol and
Analytical Method Transfer Datasheet cum report after assign a protocol
number to it and review.
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ADL and QA (TU)
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Demonstrate the analytical method to the
analyst of the QC by analyst of the ADL.
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Analyst of ADL
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Share any specific or critical information
related to the method from the QC by the ADL.
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Analyst of ADL
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Repeat the analysis using the same sample.
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Analyst of QC independently in presence of
analyst of ADL.
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Study the parameters to be transfer to QC as
per protocol.
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ADL and QC
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Compile the results obtained by both the
analysts in Datasheet cum Report.
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ADL and QC
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Check for the data to comply with the
acceptance criteria.
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ADL and QC
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Certification shall be done after completion of
Technology Transfer
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QC, QA(RU), QA (TU) and Head (RC)
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4.10.2.2.
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If the acceptance criteria do not meet in
case of collaborative study, Head of QC shall analyze the data to look for
any ambiguity. The method can then be transferred with proper justification.
If failure still persists, QC shall perform tests again. Sample conditions
should also be evaluated to check possible degradations.
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4.10.2.3.
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For failure, where analysis involves only
Direct Transfer, the analysis shall be repeated using the same batch by the
Transfer unit person at QC location.
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4.10.2.4.
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If the method does not meet the acceptance criteria even after the
repeat analysis, the follow up action shall be decided by Head of QC.
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4.10.3.
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Co-validation study between two or more laboratories
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4.10.3.1.
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The laboratory that performs the validation of an analytical procedure
is qualified to run the procedure.
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4.10.3.2.
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The transferring unit can involve the receiving unit in an
interlaboratory co validation including them as a part of the validation team
at the transferring unit and thereby obtaining data for the assessment of
reproducibility.
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4.10.3.3.
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This assessment is made using a preapproved transfer or validation
protocol that provides the details of the procedure, the samples to be used,
and the predetermined acceptance criteria.
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4.10.4.
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Revalidation
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4.10.4.1.
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Revalidation or partial revalidation is acceptable approach for
transfer of a validated procedure.
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4.10.4.2.
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Validation shall be done as per current receiving unit SOP.
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Sr. No.
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Actions
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Responsibility
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Perform method validation at the QC.
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QC
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Prepare Analytical method transfer protocol and
Analytical Method Transfer Datasheet cum report after assign a protocol
number to it and review.
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QC and QA (RU)
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Perform the validation parameter as per QC SOP
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QC
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Approve the validation protocol and
report
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QA(RU)
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Check for the data to comply with the
acceptance criteria.
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QC and QA (RU)
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Certification shall be done after completion of
validation and according to that technology transfer document to be
prepared
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QC and QA (RU)
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4.10.5.
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Transfer Waiver
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4.10.5.1.
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The conventional transfer of analytical method may be omitted under
certain circumstances. In such instance, receiving unit is considered to be
qualified to use the analytical test procedures without comparison and
generation of interlaboratory comparative data. The following examples give some scenarios that may justify the waiver
of transfer of analytical procedure:
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4.10.5.1.1.
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The new product’s composition is comparable
to that of an existing product and/or the concentration of active ingredient
is similar to that of an existing product and is analyzed by procedures with
which the receiving unit already has experience.
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4.10.5.1.2.
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The analytical procedure being transferred
is described in the USP–NF, and is unchanged. Verification should apply in
this case.
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4.10.5.1.3.
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The analytical procedure transferred is the
same as or very similar to a procedure already in use.
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4.10.5.1.4.
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The personnel in charge of the development,
validation, or routine analysis of the product at the transferring unit are
moved to the receiving unit.
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4.10.5.2.
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If eligible for transfer waiver, the receiving unit should document it
with appropriate justifications by Receiving unit.
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4.11.
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Parameters to be study
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4.11.1.
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Assay
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Parameters
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HPLC
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System Suitability
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As per STP or as per
technology transfer protocol.
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Analysis of samples
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Six Test Preparation as
specified in individual STP or as per technology transfer protocol.
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Acceptance criteria
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1) The results obtained
by both the laboratory should comply as per Analytical Method Transfer
protocol.
2) Relative Standard
Deviation (RSD) of % Assay of six preparations performed at transfer and
receiving units should not be more than 2.0% or as per Analytical Method
Transfer Protocol.
3) Mean at Receiving
unit within ± 3% of mean at Transfer unit.
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4.11.2.
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Related Substances\Chiral purity\Residual solvents:
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Parameters
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High Performance Liquid Chromatography (HPLC) /
Gas Chromatography (GC)
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System Suitability
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As per STP or as per
technology transfer protocol
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Analysis of samples
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Six Test Preparation as
specified in individual STP or as per technology transfer protocol.
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Acceptance criteria
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For Related Substances/Chiral purity (By HPLC):
1)The results obtained
by both the laboratory should comply as per Analytical Method
Transfer Protocol.
2) Difference between
lowest value and highest value of six results should not be more than 0.03%
absolute for individual impurities for related substances and chiral
purity.
3) Difference between
lowest value and highest value of six results should not be more than 0.05%
absolute for total impurities for related substances.
4) Difference between
lowest value and highest value of twelve results (six each performed at
Transfer and Receiving Unit) should not be more than 0.05% absolute for
individual impurities for related substances and chiral purity.
5) Difference between
lowest value and highest value of twelve results (six each performed at ADL
and QC) should not be more than 0.05% absolute for total impurities for
related substances.
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Acceptance criteria
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For Related Substances
(By TLC):
1) The results obtained
by both the laboratory should comply as per Analytical Method Transfer
Protocol.
2) RSD of Rf value for
individual (known and unknown) impurity from six test preparations each
performed at transfer and receiving units should not more than 15.0%.
3) RSD of Rf value for
individual impurity from twelve test preparations performed transfer and
receiving units should not more than 15.0%.
4) RSD of Rf value for
active ingredient from six test preparations each performed at transfer and
receiving units should not more than 15.0%.
5) RSD of Rf
value for active ingredient from twelve test preparations performed
transfer and receiving units should not more than 15.0%.
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For Residual solvents:
1) The results obtained
by both the laboratory should comply as per technology transfer protocol.
2) RSD of Residual
solvent of six preparations performed at each of the testing laboratories
should not be more than 15.0% by GC and 5.0% by HPLC or as per technology
transfer protocol.
3) RSD of Residual
solvent of twelve preparations (six each performed at ADL and QC) should
not be more than 15.0% by GC and 5.0% by HPLC or as per technology transfer
protocol.
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4.12.
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Report evaluation by Collaborative study by Direct/Indirect Method
Transfer
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Sr. No.
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Actions
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1
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Review and approve the
results obtained.
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2
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Get the results at the
QC for evaluation and comparison.
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3
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Check for the data to
comply with the acceptance criteria.
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4
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Certify technology
transfer activity after completion.
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5.
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RELATED DOCUMENTS
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5.1.
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Nil
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6.
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REFERENCES
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6.1.
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Nil
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