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 Pharmaceutical Guidance 

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January 4, 2023

Hold Time StudyGuidance

Pharmaceutical Protocol

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Hold Time Study Protocol

1. Objective \ Scope

1.1. Hold time study data shall give the assurance

of the maximum allowable hold times for bulk
and in-process drug products. Generally, one lot
can be used for validating hold times if any
inconsistency results were observed then another
two lots can be used for this study.

1.2. Although there are no specific regulations or

guidance documents on bulk product hold times,
GMP dictates that hold times should be validated
to ensure that in-process and bulk products can
be held, pending the next processing step,
without any adverse e!ect on the quality of the
material. Hold time study provides the re-
assurance of the quality at each in-process stage.

1.3. Although there are no specific regulations or

guidance documents on bulk product hold times,
GMP dictates that hold times should be validated
to ensure that in-process and bulk products can
be held, pending the next processing step,
without any adverse e!ect on the quality of the
material. Hold time study provides the re-
assurance of the quality at each in-process stage.

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1.4. Although there are no specific regulations or

guidance documents on bulk product hold times,
GMP dictates that hold times should be validated
to ensure that in-process and bulk products can
be held, pending the next processing step,
without any adverse e!ect on the quality of the
material. Hold time study provides the re-
assurance of the quality at each in-process stage.

1.5. Although there are no specific regulations or

guidance documents on bulk product hold times,
GMP dictates that hold times should be validated
to ensure that in-process and bulk products can
be held, pending the next processing step,
without any adverse e!ect on the quality of the
material. Hold time study provides the re-
assurance of the quality at each in-process stage.

2. Responsibilities

2.1. Validation O"cer:

To prepare protocol and report.

Sampling as per the approved protocol.
Conclude the result.

2.2. Quality Control:

Review of Protocol and report.

To analyze the hold time study samples as
per the approved protocol and report the
results.

2.3. Quality Control (Microbiology):

Review of Protocol and report.

To analyze the hold time study samples as
per the approved protocol and report the
results.

2.4. Head – Quality Assurance:

Approval of protocol and result

3. Hold time consideration

3.1. Granulation Solutions, Coating Solutions:

Typically, if these in-process products are used

within 24 hours of manufacturing, no bulk holding
timeTostudies are deemed necessary. An in-process
analyze the hold time study samples as
product that is held for longer than 24 hours
per the approved protocol and report the
should be monitored for physical characteristics
results.
and microbial contamination.

A coating solution should be held for the defined

hold period. At the test points, a sample should
be taken from the storage container and tested.
The results obtained should be compared with
the initial data of the solution control sample
results.

3.2. Powder Blends, Granules:

In-process products such as Powder blends and

granules can be held for up to 30 days from the
date of production without being retested prior to
use. An in-process product that is held for longer
than 30 days should be monitored for hold time
study under controlled storage conditions for the
length of the holding period.

At the test points, a sample should be taken from

the storage container and tested. The results
obtained should be compared with the initial data
of the core tablet and pellet control sample
results.

3.3. Core Tablets:

In-process products such as core tablets and

extended-release pellets can be held for up to 30
days from the date of production without being
retested prior to use. An in-process product that
is held for longer than 30 days should be
monitored for hold time study under controlled
storage conditions for the length of the holding
period.

At the test points, a sample should be taken from

the storage container and tested. The results
obtained should be compared with the initial data
of the core tablet and pellet control sample
results.

3.4. Bulk Tablets and Capsules:

Bulk tablets and capsules can be held for up to 30

days from the date of production without being
retested prior to use. A bulk product that is held
for longer than 30 days should be monitored for a
hold time study under controlled storage
conditions for the length of the holding period.

At the test points, a sample should be taken from

the storage container and tested. The results
obtained should be compared with the initial data
of the tablet and capsule control sample results.

3.5. Oral Liquids and Semi-Solids:

(Suspensions, Creams, and Ointments).

Typically, liquid and semi-solid dosage form

products should be held for no more than 5 days
without a hold time study. Full-scale batches
should be used for these studies.

Samples should be taken from the holding vessel

after transfer from the manufacturing vessel, and
again at the completion of the holding period.
Multiple samples should be taken at each time
point if holding can impact product uniformity.
Samples would be taken to prove the product
uniformity of actives and preservatives.

4. Hold time stages

The hold time study for the product shall be

carried out in three batches. The validation o"cer
shall collect the sample as per protocol during the
manufacturing of the planned batches.

The selection of hold time study conditions is very

important for starting the hold study. These
conditions are the same as the manufacturing
area/hold area conditions, so these conditions are
may vary from product to product. Based on the
manufacturing process of the dosage forms hold
study stages can be decided. Hold study’s
required stages are summarized in the table.

5.Teststobeconsidered

Proposed HoldTimeStudyTime
HoldTime
StudyRequired
Hold
Points TestsRequired
Time
CoreTablets(DirectCompression/DryGranulation)
Granules 45days Initial,15,30and45days Description,LossonDryingand
Assay

Lubrication 45days Initial,15,30and45days LossonDrying,ContentUniformity,

ParticleSize.Bulk/TappedDensity
Initial,30,45,60and90 Description,Hardness,Thickness,
CoreTablets 90days days
Friability,Disintegration,Dissolution.
Assay
CoreTablets(WetGranulation)
Initial,2,5,8hours
Bindersolution 8hours Incaseofstarch:initial.2 Appearance
5hours
DriedGranules 45days Initial.15.30and45davs DescriptionandLOD
Lubrication 45days Initial,15,30and45days LossonDrying,ContentUniformity,
ParticleSize,Bulk/TappedDensity
Description,Hardness,Thickness,
Initial,30,45,60and90
CoreTablets 90days Friability,Disintegration,Dissolution,
days
Assay
CoatedTablets(DirectCompression/DryGranulation)
Granules 45days Initial,15,30and45days Description.LODandAssay

Lubrication 45days Initial,15,30and45days LossonDrying,ContentUniformity,

ParticleSize,Bulk/TappedDensity
Initial,30,45,60and90 Description,Hardness,Thickness
CoreTablets 90days days
Friability,Disintegration,Dissolution,
Assay

CoatingSolution 72hours
Initial,12,24,36,48,60 PhysicalAppearance,Specific
and72hours Gravity.Viscosity,Sedimentation,pH
Initial,30,45,60and90 Description,Hardness,Thickness
CoatedTablets 90days days
Friability,Disintegration,Dissolution,
Assav
CoatedTablets(WetGranulation)
Initial,2,5,8hours
Bindersolution 8hours Incaseofstarch:initial,2 Appearance
5hours

DriedGranules 45days Initial,15,30and45days DescriptionandLOD

Lubrication 45daysInitial,15,30and45days LossonDrying,ContentUniformity,

ParticleSize,Bulk/TappedDensity
Description,Hardness,Thickness,
Initial,30,45,60and90
CoreTablets 90days Friability,Disintegration,Dissolution,
days
Assav

Initial,12,24,36,48,60 PhysicalAppearance,Specific
CoatingSolution 72hours and72hours Gravity,Viscosity,Sedimentation,pH

CoatedTablets 90days Initial,30,45,60and90 Description,Hardness,Thickness,

days Friability,Disintegration,Dissolution.
Assay
Dispersible/OrallyDisintegratingTablets
Granules 45days Initial,15,30and45days LossonDrying,ContentUniformity,
ParticleSize,Bulk/TappedDensity
Compressed Initial,30,45,60and90 Description,Hardness,Thickness
Tablets 90days days Friability,Disintegration,Dissolution,
Assay
Capsules(PowerFilling)
Lubrication 45days Initial,15,30and45days LossonDrying,ContentUniformity,
ParticleSize,Bulk/TappedDensity
Filledcapsules 90days
Initial,30,45,60and90 Description,Disintegration,
days Dissolution,Assay.
Capsules(PelletsFilled)
DrugPellets 45davs IInitial.15.30and45davs Descriptionandassay.
Lubrication 45days Initial,15,30and45days LossonDrying,ContentUniformity,
ParticleSize,Bulk/TappedDensity
Filledcapsules 90days Initial,30,45,60and90 Description,Disintegration,
days Dissolution,Assay
Liquids(Syrups,OralSolutions,Suspensions)
Un-filtered Description,pH,SpecificGravity,
solution
7days 1,2,5and7days AssayandMicrobialLimit
Filteredsolution 7days 1,2,5and7days Description,pH,SpecificGravity,
AssayandMicrobialLimit
Ointments/Gels/Creams
Bulkstage 72hours Initial,12,24,36,48andDescription,pH,SpecificGravityand
72hours assav

6. Conclusion :

6.1. The conclusion should state whether the

outcome of the activity was successful or not.

7. Revalidation Criteria:

7.1. The hold time study shall be performed again

in case of any major change in the product
specification.

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