Sop for Hold time study
This Document describes (Standard Operating procedure) SOP for hold time study for establishment of hold time of products at various stages such as lubricated granules / blend, compressed tablets, coated tablets and filled capsules, Ointment shall be stored before proceeding for the next stage .
Sop for Hold time study
I. Purpose & Scope:
- The Purpose of this SOP is to lay down the procedure for establishment of hold time of products at various stages such as lubricated granules / blend, compressed tablets, coated tablets and filled capsules, Ointment shall be stored before proceeding for the next stage.
- This procedure is applicable for Production and Quality assurance Department personnel for stagewise establishment of hold time for drug products.
II. Responsibilities:
- All production and Quality assurance personnel’s shall be responsible to follow and implement this SOP.
III . Introduction and Procedural Part :
PROCEDURE:
- Lubricated granules, compressed tablets, coated tablet for Tablet Dosage form shall be placed in double polybag and stored in SS container with lid.
- Stimulation of worst case condition:
- Container: By keeping hold time sample into In-Process Container (IPC) which is used for routine storage of bulk granules/compressed tablet/coated tablet.
- Exposure surface: The exposure surface area of stimulated worst case condition for hold time sample shall be equivalent with routine IPC container.
- Environmental condition: Temperature and humidity shall be stimulated as per labeled storage condition.
- Stimulation location: In respective quarantine area
- Capsule Blend, Filled Capsule for Capsule Dosage form, shall be placed in double polybag and stored in SS container with lid; Ointment dosage form shall be stored in SS container with lid in respective Quarantine area by stimulating label claim storage condition.
- Lubricated granules, compressed tablets, coated tablet for Tablet Dosage form shall be placed in double polybag and stored in SS container with lid in respective Quarantine area by stimulating label claim storage condition.
- Hold Time Study samples shall be collected as per their respective Hold Time Study Protocols.
- Sampling of various stage, sampling procedure shall be followed as per respective SOP
- Stages, Period of Storage, Storage Conditions and the Tests that shall be performed are enumerated as below:
| Stages | Period | Storage
condition |
Tests to be Performed
(but not limited to) |
| For Tablet dosage form | |||
| Binder solution | Initial, 02 hrs 05 hrs and 8 hrs
Starch-Initial, 02 hrs and 5 hrs |
As per product manufacturing condition | Microbial test |
| Lubricated Granule/
blend |
Initial, 7 days, 15 days, 30 days and 45 days | As per product storage condition | Description, LOD, Assay, Moisture content/ LOD and Microbial testing |
| Compressed, (Uncoated) | Initial, 30 days, 45 days, 60 days and 90 days | As per product storage condition | Description, Hardness, Friability, DT, Dissolution , Related substances, Assay, Uniformity of dosage form and Microbial test |
| Coating
Solution |
Initial, 24, 48 Hrs | As per product manufacturing condition | Appearance, pH,
Microbiological Tests |
| Coated | Initial, 30 days, 60 days and 90 days | As per product storage condition | Description, DT, Assay, Dissolution, Related Substance, Uniformity of dosage form and Microbiological test |
Microbial test- Total bacterial count, Mold and yeast, Pathogen-Ecoil, S-aureus, Ps.aeruginosa, Salmonella Spp.
| Stages | Period | Storagecondition | Tests to be Performed
(but not limited to) |
| For Hard Gelatin Capsule Dosage Form | |||
| Blend
|
Initial, 15 days, 30 days | As per product storage condition | Appearance, Moisture content/ LOD, Assay and Microbiological Tests |
| Filled | Initial, 15 days, 30 days, 45 days | As per product storage condition | Description, Disintegration, Assay, Dissolution, Microbiological Test |
| For Ointment | |||
| Bulk | Initial, 24 Hrs., 48 Hrs. and 72 Hrs. | As per product storage condition | Appearance, wt./ml, Assay, pH, Microbiological Test. |
Microbial test-Total bacterial count, Mold and yeast, Pathogen-Ecoil, S-aureus, Ps. aeruginosa, Salmonella Spp.
- Test performed shall be as per the protocol and compile the results for review.
- The outer container of this study shall be labeled with product hold time study label as per annexure – I
- Schedule of this study shall be maintained for sample kept on, withdrawal due on, actual withdrawal on, withdraw by etc as per annexure – II for hold time sample withdraw schedule.
- If results are out of limit at any stage/ period of testing as per specification then investigation shall be done.
- On completion of the study, Head QA shall review the data and conclude the result.
- Conformance to acceptance criteria of the study interval shall be used to assign the hold time of the manufacturing stage within which next process is to be taken.
- After this study, conformance hold time shall be specified in respective batch manufacturing record through change control proposal note.
ANNEXURE :
| Annexure No | Format Name |
| Annexure I | Product Hold Time Study Label |
| Annexure II | Hold Time Study Sample Withdrawal Schedule |
Annexure I
|
Status Label:
- Label Size : Length : 12.00 cm, Width : 8.5 cm
- Label used by QA department which is in white color background.
Quality assurance Personnel should affix product hold time study label on outer container.
Annexure II
HOLD TIME STUDY SAMPLE WITHDRAWAL SCHEDULE
| Product Name: | |
| Batch No.: | Batch Size: |
| Mfg Date: | Exp Date: |
| Average Weight: | Stage: |
| Sample put on for Hold time study (Date): | |
| Sr. No. | Sample Withdrawal schedule interval | Sample Withdrawal due on (Date) | Sample Withdraw on (Date) | Withdraw Sample Qty. | Study sample withdrawal by QA | Sign. |
