SOP on In-process sampling of semi-finished product
Objective:
To lay down the procedure for in-process sampling of semi finished drug product.
Scope:
This procedure is applicable to the in-process sampling of semi-finished drug product in formulation plant of Pharmaceutical company.
Responsibility:
IPQA personnel are responsible for collecting in-process semi finished product samples.
Production personnel are responsible for intimation to IPQA for collection of in-process semi finished samples from the production process.
Accountability:
Head – QA shall be accountable for compliance of the SOP.
Procedure:
Sampling of In-process semi finished products (Tablets, Capsules, Dry syrup):
In-process semi finished products can be classified into different categories, based on stages of processing:
- Powder blend.
- Core Tablets.
- Coated Tablets.
- Filled capsules.
Note: Next step shall be carried out only when the result of the In-process semi-finished products meets the specified criteria.
Powder blend:
On completion of the process, Production personnel shall intimate IPQA personnel for collecting the samples.
IPQA shall collect the samples from three different layers (locations) (top, middle and bottom) using suitable sampling aid and send composite samples to QC along with duly filled sample intimation slip.
For exhibit / validation batches the samples collected according to the sampling plan given in protocol by IPQA person at each stage.
For blend uniformity testing, the samples collected from the blender shall be 1x to 3x of the quantity equivalent to each dose unit.
Under Test label shall be affixed on containers by IPQA.
100 grams sample shall be collected for chemical testing.
Tablets and capsules:
On starting of compression process for tablets and the filling process for capsules, Production personnel shall intimate IPQA personnel for collecting the samples.
IPQA shall start collecting samples from initial, middle and end of the batch during the operation. Samples shall represent the whole batch manufacturing operation.
For chemical analysis (physical and chemical parameters), samples shall be collected as per the sampling plan mentioned in Table-1.
For exhibit / validation batches the samples are collected according to the sampling plan given in protocol by IPQA person at each stage.
Samples shall be sent to QC with intimation form duly filled by IPQA.
Dry Syrup:
On starting of filling and sealing operation, Production personnel shall intimate IPQA, for collecting the semi-finished product samples of dry syrup.
IPQA shall start collecting samples from initial, middle and end of the batch and after any break down of the machine operation for which the filling operation is stopped for more than 30 minutes. Samples shall be representative of the whole batch.
For physical and chemical testing, separate samples shall be collected as per the sampling plan mentioned in Table-1.
Dry Powder Injection:
On starting of filling and sealing operation, Production personnel shall intimate IPQA, for collecting the semi-finished product samples.
IPQA shall start collecting samples from initial, middle and end of the batch and after any break down of the machine operation for which the filling operation is stopped for more than 30 minutes. Samples shall be representative of the whole batch.
For chemical, microbiological and endotoxin testing, separate samples shall be collected as per the sampling plan mentioned in Table-2.
For exhibit / validation batches the samples shall be collected according to the sampling plan given in protocol by IPQA person at each stage.
Samples shall be sent to QC with intimation form duly filled by IPQA with proper label.
Table: 1
In-process Sample Quantity for physical and chemical analysis for Tablets, Capsules, Dry syrup
| S.No. | Product name | Physical & Chemical analysis | |
| 1 | Oral Suspension (Dry syrup) | 40 bottles | |
| 2 | Tablets | 120 tablets | |
| 3 | Capsules | 60 capsules | |
Table: 2
In-process Sample Quantity for Physical and Chemical analysis for Injectable product
| S.No. | Product name | Strength | Chemical analysis Quantity (Vials) |
| 1 | Powder for injection
|
0.25 g | 65 |
| 0.5 g | 55 | ||
| 0.75 g | 50 | ||
| 2 | 1.0 g | 45 | |
| 1.5 g | 45 |
List of Annexures and Formats:
Sample Intimation Slip – Annexure – I
References (if any):
Not applicable.
Reason for revision:
New SOP
Abbreviations
IPQA: In process Quality Assurance
Annexure – I
Sample Intimation Slip (semi-finished product)
(Blend, Core / Coated Tablets, Filled Capsules, Oral Dry syrup, Dry powder for injection)
| From: Production:_____________ | To: Quality Assurance Dept. | |||
| Initiated by: Production: _________ | Date / Time:_____________________ | |||
| Intimation received by: (QA)____________ | Date / Time:_____________________ | |||
| Product Details (To be filled by Production): | ||||
| Product Name:______________________ | Stage:________________ | |||
| Batch No._________________________ | Batch Size:_________________________ | |||
| Mfg. Date:_________________________ | Exp. Date:__________________________ | |||
| Sampling Details (To be filled by QA): | ||||
| Sampled by (QA):_________ | Date of Sampling: ________Qty. Sampled (g / units.):________ | |||
| Analysis required (To be filled by QA): | ||||
| Test(s): Blend assay, Blend uniformity, Water (KF), LOD, DT, Dissolution, Reconstitution, Hardness, Friability, Av tablet wt; Av Capsule fill wt; Av Bottle / Vial Fill wt; Leakage, | ||||
| Test Results (To be filled by QC): | ||||
| Remarks (by QC): The sample conforms/does not conform as per ______________ Specification | ||||
| Analyzed by/(Sign / Date) | Manager – Q.C./(Sign / Date) | |||
| Recommendation by QA (If sample does not conform)____________________________________
Manager – Q.A./(Sign / Date) |
||||
Sample Intimation Slip (Semi-finished product)
Stage: (Blend, Core / Coated Tablets, Filled Capsules, Oral Dry syrup, Dry powder injection)
| From: Production:_____________ | To: Quality Assurance Dept. | |||
| Initiated by: Production: _________ | Date / Time:_____________________ | |||
| Intimation received by: (QA)____________ | Date / Time:_____________________ | |||
| Product Details (To be filled by Production): | ||||
| Product Name:______________________ | Compression /fill weight:______________ | |||
| Batch No.:_________________________ | Batch Size:_________________________ | |||
| Mfg. Date:_______________ | Exp. Date:__________________________ | |||
| Sampling Details (To be filled by QA): | ||||
| Sampled by (IPQA)
(Name/sign) :________/_____ |
Date of Sampling: ________Qty. Sampled (g / units.):________ | |||
| Samples to be sent to: Micro / QC | ||||
| Test Results (To be filled by QC): | ||||
| A.R No.: | ||||
| Assay:_____________ (Limit _________ ) | Dissolution: Min____ Max____ (limit _______) | |||
| LOD/ Water:___________ (Limit ________ ) | pH ________________ (Limit __________ ) | |||
| Other: | ||||
| Remarks (by QC):The sample conforms / does not comply as per Specification No.___________ | ||||
| Analyzed by
(Sign / Date) |
Manager – Q.C.
(Sign / Date) |
|||
| Recommendation by QA (If the sample does not conform)________
Manager – Q.A./(Sign / Date) |
||||
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