To lay down a procedure for Sampling of Inprocess materials and Finished products.
This standard operating procedure is applicable to pharmaceutical formulation plant for the sampling of In process materials and finished products for QC analysis. This SOP shall also be applicable for sampling of Control/Reserve Samples and Stability Samples.
3.1 Officer/Executive IPQA: Sampling of Inprocess materials and finished products, control / reserve samples and stability samples.
3.2 Head, QA shall be responsible for implementation and compliance of the SOP.
4.0 Abbreviations and Definitions
BMR : Batch Manufacturing Record
S.S. : Stainless Steel
Inprocess Materials : The samples which are drawn during manufacturing process for analysis as per BMR
IPQA : Inprocess Quality Assurance
5.1 Head / In charge, Production or his/her designee shall generate the Analytical Request/ Report (Annexure-I), requesting IPQA for sampling of Inprocess material, Finished Products, Control Samples and Stability Samples.
5.1.1 The Analytical Request/Report shall consist of Doublet of sheets first in white colour and second in yellow colour.
5.1.2 The details of sampling shall be filled on the white sheet with carbon papers in between sheets duplicating the information on each sheet.
5.1.3 Both sheets shall be forwarded to QC along with the sample.
5.1.4 QC shall record the results / observations on the white sheet and shall retain the yellow sheet for its future reference.
5.1.5 The white sheet shall be sent to production which shall be attached in BMR.
5.1.6 IPQA Personnel shall record the details of product sent to QC for testing purpose in the register maintained as per Annexure-V.
5.2 Sampling of In-process Materials
5.2.1 After receiving the Analytical Request/Report (Annexure-I) from production, IPQA person shall ensure that BMR should be completed for all aspects up to the stage for which sampling has to be done.
5.2.2 Ensure that all the containers/Bins shall be properly labelled with Product Name, Batch No., Manufacturing Date, Gross Wt., Tare Wt., Net wt., Checked by and date, Container Number/Bin Number and Total number containers and Stage of the process.
5.2.3 Sampling of granules shall be done with sampling rods having sampling port of appropriate size and length .Sample for granules shall be taken from the center of bin for top, middle and Bottom layer. The sample shall be pooled before sending to QC analysis.
5.2.4 IPQA personnel shall collect the quantity of samples required for analysis as per annexure-VI, using sampling rods of appropriate size and length.
5.2.5 IPQA person shall paste “SAMPLED” label (Yellow in colour) (Annexure-II) with date and signature on the containers selected for the sampling and reseal the containers tightly after sampling.
5.2.6 IPQA person shall submit the sample after affixing label along with Analytical Request/Report (Annexure-I) to QC for analysis. After approval of samples ‘APPROVED’ label (Green in colour) (Annexure-II) with date and sign of IPQA person shall be pasted on all the containers of the batch.
Sampling of Tablets and Capsules
5.2.7 When the total number of containers are 4 or less than 4, collect samples from each container and pool. When the total number of containers are more than 4 collect samples atleast from √n + 1 number of containers and pool (where n is total number of containers).
Note: 1) Ensure that samples are collected from 1st and the last container.
2) In case of coated tablets, collect samples individually from all the lots and from each container.
5.2.8 Collect the sample in the suitable containers or equivalent to avoid any spillage of the material.
5.2.9 Mention Lot No. / Batch No. separately on the ‘SAMPLED’ label (Annexure-II), if required.
Sampling of Liquid Orals
5.2.10 Mix the bulk for 5 minutes.
5.2.11 Take the sample with the help of clean sampling rod for top, middle and bottom layer. The sample shall be pooled before sending to QC for analysis.
5.2.12 The usage of sampling rod shall be recorded as per Annexure-IV.
Sampling of Gel/Ointment/Cream
5.2.13 Take one cleaned container with lid, of appropriate size / capacity.
5.2.14 Open the lid.
5.2.15 Draw the sample from all the storage containers with the help of an appropriate sampling aid (with Suction Pump).Transfer the sample to the container and close the container with lid.
5.3 Sampling of Finished Products
5.3.1 Sampling of finished products shall be carried out online during packaging operations.
5.3.2 IPQA shall sample the quantity required for analysis as per annexure-6.
5.3.3 Select and pick the samples randomly from the packaging line over the period of packaging operations at different intervals.
5.3.4 IPQA person shall submit the sample along with Analytical Request/Report (Annexure-I) to QC for analysis.
5.4 Sampling of Control Samples
5.4.1 The control samples shall be taken online over the entire period during packaging operations or randomly selected after completion of packaging operations.
5.4.2 IPQA person shall take twice the quantity of finished product sample sent for analysis as control sample and shall mention the sampled quantity in the BMR.
Note: For export, the control sample quantity shall be the same as that of finished product sent to QC for analysis
5.4.3 Enter the drawn quantity of finished product as control sample in ‘Control Sample Sampling Record’ (Annexure-III).
5.4.4 IPQA personnel shall affix “Control Sample” stickers on samples (Annexure-II).
5.4.5 The control samples shall then be placed in the control sample room.
5.4.6 Control samples shall be sampled and stored in the same pack style as that of the finished good.
5.5 Sampling of Stability Samples
5.5.1 IPQA shall withdraw the stability samples online over the entire period during packaging operations as and when required.
5.5.2 The quantity of stability samples shall be as per the stability protocol of individual product.
5.5.3 IPQA shall forward the stability samples to the Incharge, Stability Cell – QC for initiation of stability.
Note: – Samples of different stages of different dosage form shall be collected as per sampling quantity data (Annexure-VI).
6.0 Forms and Records
6.1 Analytical Request/Report : Annexure-I
6.2 Formats of Labels : Annexure-II
6.3 Control Sample Record : Annexure-III
6.4 Sampling Rod Usage Log Book : Annexure-IV
6.5 Product sampling record : Annexure-V
6.6 Sampling Quantity Data : Annexure-VI
7.1 Master Copy – Documentation Cell (QA)
7.2 Controlled Copies – Production, Quality Control, Stores, Quality Assurance
|Date||Revision Number||Reason for Revision|