To lay down the procedure for Sampling of Active Pharmaceutical Ingredient (API) and Intermediates.
1.0 PURPOSE:
1.1 To lay down the procedure for Sampling of Active Pharmaceutical Ingredient (API) and Intermediates.
2.0 SCOPE:
2.1 This procedure is applicable for all API and Intermediates.
3.0 RESPONSIBILITY:
3.1 Chemist – Quality Control.
3.2 Section Head - Quality Control.
3.3 Chemist- Microbiology
3.4 Chemist- IPQA
4.0 ACCOUNTABILITY:
4.1 Head - Quality Control.
5.0 PROCEDURE:
5.1 Upon receipt of “sampling request” from manufacturing department, sampling chemist– IPQA shall check the details on the request.
5.2 Chemist– IPQA shall enter the details in the Inward register as per the sampling request (Refer Format no. XXXXX-F01 for API and XXXXX-F02 for Intermediates).
Sequential activities of Sampling Chemist.
5.3 Shall take the Sampling request, Sampling devices (such as Glass sampler, Scoop etc.), Personnel safety devices (such as Hand gloves, Goggles, Nose mask etc.) and sample collection polythene bags (for solids) or glass bottles (for liquids) from Quality Control laboratory.
5.4 Shall check the quarantine labels on the containers with respect to sampling request. Any discrepancy shall be immediately informed to production in-charge to resolve it.
5.5 Shall wear the safety devices and open them.
5.6 Shall ensure cleanliness of the sampling devices and mix the contents thoroughly with in the container by sampling scoop (for solids) or by glass sampler (for liquids).
5.7 Shall sample from all the containers in such a way that the total quantity shall be sufficient for three complete analysis (approximately 120 g for API and 60 g for intermediates, If sieve analysis and microbial analysis is required extra 30 g for each shall be drawn).
5.7.1 Quantity justification for API:
30 g for chemical & instrumental analysis
60 g for retention sample (30 g x 2)
30 g for Bulk density
30 g for Sieve analysis (If required)
30 g for Microbial analysis (If required)
5.7.2 Quantity justification for Intermediates:
20 g for chemical & instrumental analysis
40 g for retention sample (only for solids)
5.8 Shall collect the sample separately for each container in LDPE self sealed polythene bag (for solids) or in glass bottle (for liquids) and close the sample containers immediately.
5.9 Shall close all the containers.
5.10 Shall enter the observations during sampling in the “Sampling Observation sheet
5.11 Shall bring all the individual samples to IPQA and shall check the physical appearance and nature of the individual samples.
5.12 Shall blend (in case of individual samples are identical) all the samples and make a composite sample and hand over to QC.
5.13 Upon receipt of sample QC-Chemist divide this into different parts as per the requirement. Use one part for analysis and two parts for retention sample. Analysis part subdivided into 5 parts and hand over to concerned sections i.e Wet lab, HPLC, GC, IR&PS as well as Microbiology(where ever applicable)
5.14 Shall keep the sample for analysis in the respective trays labeled as “API under analysis” “Intermediates under analysis”.
5.15 Shall keep the sample for retention in the “Retention sample drawer”.
5.16 Used sample devices shall be cleaned as per the SOP No.: xxxxx.
5.18 Sampling frequency for microbial analysis:
5.18.1 First 3 validated batches of the new product or new process or new premises
5.18.2 Evry first batch of the Year and Every 10th batch of the product
5.18.3 Follow the sample frequency as per Format Nos. XXXXX and
XXXXX
END OF DOCUMENT
Pharmaceutical ingredients, intermediates, quality control
