LAB-125 Sampling of Raw Materials, In-process and Bulk Finished Product

Note 1: Ensure that all sample containers are correctly labelled before taking samples.  Each sample container bears a label with the Item Number, Product Name, Lot Number, Date of Sampling and the Sampling Point from which the sample is taken if applicable.

Note 2: The samples should be taken to the QC Laboratory and registered in the “QC Laboratory Raw Material Receival Logbook” for all raw material samples; and in the “Bulk and In-Process Sample Logbook” for all In-process and bulk samples.

5.1 Raw Material Sampling (Except for 70% Alcohol Sampling)

The sampling of Raw Materials (except for 70% alcohol) is covered by the following SOP’s:

WAR-085 Sampling and Inspection of Raw & Bulk Materials”,

WAR-100 Sampling of Raw Materials in Sampling Booth”,

WAR-105 Cleaning of Sampling Booths and Implements in the Raw Materials Quarantine Store”.

5.2 70% Alcohol Sampling

5.2.1 Materials required:

500mL x 5 sterilised jars (for microbiological testing)

120mL x 1 non- sterilised jar (for chemical testing)

1 sampling thief – sterilised

70% Alcohol

Latex gloves

Texta for labelling

5.2.2 Ensure correct gowning procedures are followed as per standard procedure for  “Personal Hygiene and Clothing Policy” and “Personal Protective Equipment Policy” for entry into the manufacturing area.

5.2.3 Ensure latex gloves sprayed with 70% Alcohol are worn prior to sampling.

5.2.4 Label all sample jars with Sample Name, Batch Number, Date and Time Sampled and the Operator Name using the labelling Texta.

5.2.5 Spray the drum cap with 70% Alcohol and remove it.

5.2.6 Remove the sampling thief from the sterilisation bag and plunge into the drum ensuring the plunger of the sampling thief is down and submerged under the liquid so it fills.

5.2.7 Remove the sampling thief gently and pulling plunge up and expel the liquid into the sample jars.  Repeat this process until all sample jars are full.

5.2.8 Tighten the lids of the sample jars to prevent leaking, take the samples to the QC Laboratory and affix proper labels to the sample jars.

5.2.9 Log the chemical sample into the “QC Laboratory Raw Material Receival Logbook” for chemical testing.

5.2.10 Send the microbiological samples to the Microbiology Lab for microbiological testing.

5.3 Blend Sampling

5.3.1 Check the sampling thief to ensure that it is clean before use.

5.3.2 The operator refers to the Product Manufacturing Instructions (MI) to determine what sampling plan is to be followed.  One sample container, 49mm x 49mm Polypropylene securitainer, is filled for each sampling point required.

5.3.3 Label each sample container with the following information: Item Code, Product Name, Batch Number, Sample Position, Signature and Date.

5.3.4 Ensure the plunger of the sampling thief is fully down before inserting the thief into the blend at the required position, as per MI, in the blender and to the required depth.

5.3.5 Holding the body of the thief at the same depth in the blend, pull the plunger up to draw some blend into the thief.

5.3.6 Withdraw the thief from the blend and while holding the thief over the sample container, press the plunger down to fill the container with sample. Note: Ensure that sample container is filled to the brim before closing the container with the lid.

5.3.7 After filling the sample container, move the plunger up and down over the blender, to remove as much excess blend material as possible before taking the next sample.

5.3.8 Press the securitainer lid firmly down on the container to achieve an airtight seal

5.3.9 Repeat Steps 5.2.3 to 5.2.8 until all required sample points have been sampled.

5.3.10 After all samples have been taken, sign and date the MI in the required position.

5.3.11 Place all the samples in a plastic bag and immediately deliver to the QC Laboratory, ensuring not to disturb the blend samples, by shaking or disturbing the samples in any way.

5.3.12 The samples are delivered to the QC Laboratory and registered in the “Bulk and In-Process Sample Logbook”.

5.3.13 The sampling thief must be cleaned as per SOP MAN-015 Factory Cleaning Procedure.

5.4 Liquid Sampling

5.4.1 Sampling is accomplished with a ladle that has been previously cleaned as per standard procedure.

5.4.2 The product is thoroughly mixed prior to sampling. The sample process is undertaken immediately after cessation of stirring.  The operator collects a sample instructed in the MI.

5.4.3 Label each sample container with the following information: Item Code, Product Name, Batch Number, Sample Position, Signature and Date.

5.4.4 Where a sample from the bottom is required, this is taken from the outlet valve at the bottom of the mixing vessel.  Approximately 200ml is flushed through the valve before taking the sample.

5.4.5 The lid is placed on the sample container immediately after the sampling.  The sample is then covered with aluminum foil (as the suspension is light sensitive) and transferred to the QC Laboratory as soon as possible.

5.4.6 The samples are delivered to the QC Laboratory and registered in the “Bulk and In-Process Sample Logbook”.

5.4.7 Used sampling tools are cleaned according to SOP MAN-010 Cleaning Responsibilities and Methods for Employees.

5.5 Ointments and Suppository Sampling

5.5.1 Sample as per MI.

5.5.2 Samples are taken using 20ml sample jar or a small stainless steel container.

5.5.3 Label each sample container with the following information: Item Code, Product Name, Batch Number, Sample Position, Signature and Date.

5.5.4 Samples are taken during the transfer from the Lexamixer to the holding tank or drums.

5.5.5 The samples are delivered to the QC Laboratory and registered in the “Bulk and In-Process Sample Logbook”.

5.6 End of Run (EOR) Tablet and Capsule Sampling

5.6.1 The Operator collects all tablet and capsule samples.

5.6.2 The size of the sample depends on the batch size and is determined according to International Standard such as ISO 9001.  A Sample equivalent to a Level II General Inspection is taken across the batch.

5.6.3 Collect an equal number of tablets or capsules from each bucket to form a representative EOR sample.  Calculate the number required from each bucket by dividing the total sample size (500, 800 or 1,250) by the number of buckets required for the job.

The net bucket weight for tablets is 12kg.  The net bucket weight for capsules is 9kg. E.g. For a Lot Size of 416,667 tablets, multiply 416,667 by the by the fill weight to calculate the weight of product to be produced.  This number then needs to be divided by 1,000,000 to convert milligrams to Kilograms.

Weight of Tablets =  416,667Tabs*480mg /Tab    = 200 KG

                                                           1,000,000

Divide the Weight of the Tablets by the net bucket weight

No. of buckets = 200 KG    = 16.7 = 17 buckets

12  Kg

Sample size is 800.  Therefore    800   = 47 tablets per bucket.

                                                                   17

5.6.4 Collect the tablets or capsules in a plastic bag.  The plastic bag is labeled with the Item Number, Product Name, Lot Number, Date, Average Weight (as determined during In-Process testing), Signature and Date and marked “EOR”.

5.6.5 The samples are delivered to the QC Laboratory and registered in the “Bulk and In-Process Sample Logbook”.

5.7 Coated Tablet and Capsule Sampling

5.7.1 The Operator collects all coated tablet samples.

5.7.2 The coating pan continually mix’s the tablets.  A representative sample is taken by transferring small scoops of tablets from the coating pan as the tablets are mixing, during the cooling down process of coating. Approximately 100grams are collected in a labeled plastic bag.

5.7.3 The plastic bag is labeled with the Item Number, Product Name, Lot Number, Date, Average Weight (as determined during In-Process testing), Signature and Date and marked “Coated”.

5.7.4 The samples are delivered to the QC Laboratory and registered in the “Bulk and In-Process Sample Logbook”.

5.8 Re-Sampling

5.8.1 Where a Raw Material, Blend, EOR, Coated or Bulk requires re-sampling the sampling steps are the same as described above for the original sample.

5.8.2 Re-sampling of a material is only permitted under certain circumstances where the integrity of the original sample is doubted, where insufficient original sample is provided to complete the required testing or for other special circumstance as authorised by the QA Manager.

5.8.3 Form-010 Sample Request Form must be completed for each re-sampling event.

5.8.4 The form must detail specifics of the re-sampling event including:

5.8.4.1 Number of samples to be taken.

5.8.4.2 Size of samples to be taken.

5.8.4.3 Location from which samples are to be drawn (original containers or new locations).

5.8.4.4 What testing is to be conducted.  (No testing other than that specified on the “Form-010 Sample Request Form” or attached Form-715 Analytical Testing Report for Non Standard Testing QA Inspection Sheet is permitted.) 5.8.4.5 Any Deviation or Laboratory investigation Report relating to the reason for re-sampling must be referred to when making the decision to re-sample.