1.0 OBJECTIVE :

To define the procedures for Sampling of all intermediate and finished products for testing the quality.

2.0 SCOPE :

This procedure is applicable for sampling of intermediate (blend/compressed tablets /coated tablets / filled capsules) and finished products (packed) during manufacturing.

3.0 RESPONSIBILITY :

IPQA  / Quality Assurance Chemist and above

4.0 ACCOUNTABILITY:

Quality Assurance Head

5.0 PROCEDURE :

5.1 Sampling plays a major role in achieving the accurate results of the analysis. Sample are representative of the whole Batch.

5.2 On completion of intermediate / finished product stage, production executive /officer will raise the intimation slip and give the intimation to IPQA chemist for sampling.

5.3 IPQA chemist will check that the BMR /BPR and log books is completed and signed up to that stage and all the manufacturing steps are followed and documented, including stage wise yields before sampling.

5.4 IPQA chemist will sample from appropriate locations, using necessary accessories like spatula, sampling bags, labels, sampling rod, mask, hand gloves & safety goggles as per necessity.

5.5 IPQA chemist should ensure that representative samples are taken in sufficient quantity, stated later in this SOP, for testing in accordance with specification.

5.6 Place the collected sample in sampling bag. Put this bag into another sampling bag bearing “IN-PROCESS SAMPLE” label with sample details.

5.7 “IN-PROCESS SAMPLE” label is computerized form printed on sticker label which contain the information.

Product Name:

Batch No. :

Batch Size:

Mfg. Date:

Exp. Date:

Sample Quantity:

Stage :

Sampled by:

Signature & Date :

5.8 Sampling of intermediate (Blend / Coating) is done using below formula.

√n+1

Where n = No. of drum/ container

Eg. √4+1

=  2+1

= 3

IPQA chemist will withdraw equal quantity of sample from 3 Containers/ drums.

5.9 Sampling of Intermediate (Compressed tablets/ Filled Capsule) and finished product is done in such a manner that (composite sample are combined into) Start, Middle and End of the batch.

5.10 Carry out sampling of  process validation sample from machine or drums as per the process validation protocol.

5.11 Carry out sampling of routine manufacturing as per this SOP.

5.12 Procedure involve in sampling stage:

Finished Final Blend :

Blends are tested for their homogeneity. Homogeneity of the blend is critical for quality of the product. The sample should be taken from at least 9 locations in the blender and make 1 composite sample by mixing in poly bag.

Area of poor blending must be covered in sampling. Corners and discharge point must have sampling location. Blender geometry should be taken into consideration during the sampling of the blender.

Collect 10 sample as mentioned below and make 1 composite sample by mixing in poly bag giving to quality control chemist or above for analysis.

Following are the sampling locations for octagonal blender.

Blend uniformity samples should be taken directly from the blender just before unloading the blend. If it is not possible to perform sampling from blender then the sample may be taken from the container after unloading.

The sampling of (Blend) is done using below formula if taken from container after unloading.

√n+1

Where n = No. of drum/ container

Eg. √4+1

=  2+1

=  3

IPQA chemist will withdraw equal quantity of sample from 3 Containers/ drums.

Collect the sample in sampling bag. Put this bag into another sampling bag bearing label of complete pool sample details.

Blend samples should be handled and weigh carefully because segregation may occur during weighing, handling and submission to Quality Control department.

Production executive /officer and IPQA chemist will sign in the BMR.

IPQA chemist will submit approximately  5 gm of blend sample to Quality control chemist along with Intimation Slip as early as possible or within 2 hours after sampling and make an entry in the In process sample register.

Affix To be cleaned label on spatula/ sampling rod and send it for washing refer as per SOP in particular area where operation is carry out.

5.13 Sampling of Compressed tablets /Coated tablets/ Filled capsules:

Compressed Tablets:

After completion of compression machine setting and in-process checking ; collect the sample 10 to 15 tablet during each in-process interval by placing the poly bag at discharge chute (LHS and RHS) and place the sample in glass bottle till the batch completed and make composite representative sample for each batch. The sample quantity of tablets may vary as per batch size, after receiving the Intimation slip from Production Officer for sampling purpose.

Coated Tablets:

After in-process checking ; collect the sample 10 to 15 tablets during each in-process interval from each coating pan after completion of 1 lots or batch and place the sample in glass bottle till the batch completed and make composite representative sample for each batch. The sample quantity of tablets may vary as per batch size after receiving the Intimation slip from Production Officer for sampling purpose.

Filled Capsules:

After completion of capsule machine setting and in-process checking collect the sample 10 to 15 capsules during each in-process interval by placing the poly bag over exit chute and place the sample in glass bottle till the batch completed and make composite representative sample for each batch. The sample quantity may vary as per batch size after receiving the Intimation slip from Production Officer.

Production Executive /Officer and IPQA Officer will sign in the BMR.

IPQA chemist will submit the sample to Quality Control chemist or above along with intimation slip and make an entry in the In process sample register.

Sampling of Finished Product/ Control Sample/ Stability Sample:

IPQA chemist shall withdraw the sample online at the time of packaging operation at different intervals and submit the sample to Quality Control chemist or above along with intimation slip and make an entry in the In process sample register.(Initial, Middle, End).(Total quantity of sample should approximately be near to the quantity mentioned in Table No. I).

Packing officer should make all the entries of Finished product sample, control sample and stability sample in the BPR.

 6.0 ABBREVIATIONS:

Abbreviation Expanded form

SOP Standard Operating Procedure

Q.A. Quality Assurance

Q.C. Quality Control

BMR Batch Manufacturing Record

BPR Batch Packing Record

gm Gram

IPQA In- Process Quality Assurance

LHS Left Hand Side

RHS Right Hand Side

7.0 ANNEXURES:

Annexure No. Title

01 Format for In process Sampling by IPQA

8.0 SOP REFERENCES

GMP Guidelines