Site icon Pharma Dekho

sop for sampling of intermediates and finished products

 

sop for sampling of intermediates and finished products

 

1.0 OBJECTIVE: 

The objective of this SOP is:
1.1 To describe the procedure for sampling of intermediates and finished products during manufacturing operations.

2.0 RESPONSIBILITIES:

2.1 Quality Assurance Officer / Executive shall be:
2.1.1 Responsible for withdrawal of samples of Intermediates and Finished products on receipt of intimation from production.
2.1.2 Responsible for sending the collected sample with Sample advice slip to Quality Control for analysis.

3.0 ACCOUNTABILITY:

Head – Quality Assurance

4.0 PROCEDURE:

4.1 Preparation:
4.1.1. On receipt of Request for Analysis from production check that the BMR is completed up to that stage and all



the manufacturing steps are followed and documented including stage wise yields.
4.1.2. Ensure availability of clean spoon, clean bottles, vials, polybags, labels etc.
4.1.3. Prepare a sample label, which should contain following information.
a. Product name
b. Batch No.
c. Mfg . Dt . Exp. Dt :
d. Stage
e. Test
f. Sampled by.
g. Date of sampling

4.1.4. Affix the label on container to be used for sampling i.e. polybag in case of powder, tablets and capsules and glass container in case of liquids.

4.1.5. Wear latex hand gloves and nose masks.
4.1.6. Ensure that all the bulk container carry ‘STAGE’ labels with correct product and batch details.

4.2 Sampling Of Intermediates (Sterile):

4.2.1 Sterile Blend sampling will be done by Quality Officer( Microbiologist ) as per SOP No: A/QA/041.

4.3 Intermediate (Non-Sterile):

4.3.1 Open the container and withdraw equal quantity of sample from all the containers to make a pool sample as quantity mentioned below.

NOTE:
Core Tablets / capsules for Dissolution test should be sent after ensuring compliance of
physical parameter against limits as mentioned in BMR.

Sr. No. Dosage Form Sample quantity (Approximately)
1. Capsules (Blend / Granules) 15.0 gm
2. Tablets   (Blend / Granules) 15.0 gm
3. Dry syrup Sugar for LOD 5.0 gm
4. Dry syrup (Blend Granules) 30.0 gm
5. Dispersible tablet (Blend / Granules) 15.0 gm
6. Core Tablets for Dissolution 20.0 No.

4.3.2 In case of bulk requiring the test of bulk density & particle size 20 gm extra sample per test shall be sent.

4.4 Non Sterile Liquids
4.4.1 Open the container and withdraw the sample with help cleaned silicon tube in clean dry glass container.
4.4.2 For light sensitive products sample container should be wrapped with Aluminium foil or black paper.
4.4.3 In case of Water for Injection collect the sample directly from solution preparation tank with help of cleaned silicon tube in cleaned glass container.
a. Sample Qty Bulk samples – 50 ml Approximately
b. Water for injection for bulk Mfg – 500 ml Approximately.

4.5 FINISHED PRODUCT SAMPLING:

4.5.1 Dry Syrup / Liquid Orals
4.5.1.1 Based on the following sample plan draw equal number of samples of filled bottles to represent start, middle and end of the filling operation so that the total numbers of sampled bottles, at the end of the batch is at least equal to the sample size required by the quality control lab.
1. Liquid Oral
a. 30ml Bottles –            10 Nos.
b. 50ml Bottles –           10 Nos.
c. 60ml Bottles –           10 Nos.
d. 100ml Bottles –        10Nos.
e. 200ml Bottles –        10 Nos.
2. Dry Syrup –               20 Nos



• In case of dry syrup requiring the test of content uniformity 10 bottles extra-shall be sent.
• In case of dry syrup requiring the microbiological test, 2 bottles extra shall be sent.

4.5.2 VIALS
4.5.2.1 In case of sterile dry powder and liquid vials draw equal number of samples from the start of filling operation

and thereafter at hourly interval till the end of the filling operation or if there any intervention so as to have requisite number of total samples indicated below
a. Sterile dry powder vials :      50 Nos.
b. Liquid vials (2ml) :              25 Nos.

4.5.2.2 The first two filled at the start of filling operation shall be sampled and thereafter-adequate number of samples

should be withdrawn at hourly intervals. Also last two units filled at the end of filling operation shall be sampled
Note:
Incase of export product, Quality Officer ( microbiologist) shall collect sample sas per SOP No: A/QA/041at aseptic area for

all API container used in filling for identification and sterility testing.

4.5.2.3 Store the collected samples in labeled container/polybag.
4.5.2.4 And send the collected sample to quality control for analysis.
4.5.2.5 Incase of Injectable products requiring the test of particulate matter as per USP, additional number of following samples should be sent.
a. Liquid vials 1ml, 2ml – 40 vials
b. Liquid vials 5ml, 10ml – 20 vials

4.5.3 TABLETS/ CAPSULES

4.5.3.1 Collect samples from the containers to make pool sample, based on following sampling plan.

No. Of containers   Containers to be sampled
0 to 5                                    vials All
6 to 15                                      5
16 & above                             ^n +1
Note:
Collect sample from containers in such a way that the sample is representative of whole batch.

 

4.5.3.2 If the coating is carried out in more than one lot, withdraw equal quantity of sample
from each lot and make pool sample.
4.5.3.2 In case of tablet / capsules requiring the microbiological test, 40 tablets/ capsules be sent.

4.5.4 AMPOULES:

4.5.4.1 The number of samples to be down shall be as follows
a. 1 ml :               125 No. per lot
b. 2 ml :              100 No. per lot
c. 3 ml :              80 No. per lot
d. 5 ml :              80 No. per lot
e. 10ml :             80 No. per lot
f. 15ml :             50 No. per lot

4.5.4.2 Incase of Injectable products requiring the test of particulate matter as per USP,
4.5.4.3 Additional number of following samples should be sent.
a. 1 ml ampoules :                             50 Nos.
b. 2 ml & 3ml ampoules :                25 Nos.
c. 5 ml, 10 ml & 15 ampoules :      20 Nos.

4.5.4.4 For aseptically filled ampoules / vials.
4.5.4.5 The first two units filled at the start of filling operation shall be sampled.
4.5.4.6 Thereafter adequate number of samples should be withdrawn at hourly intervals and units filled at the end of filling operation shall be sampled
4.5.4.7 Store the collected samples in labeled containers/ polybag.
4.5.4.8 Send the filled containers to Quality Control Laboratory. Ensure that they are not less than required quantity.
4.5.4.9 For terminally sterilized ampoules
4.5.4.10 Draw equal number of samples from upper, middle and lower shelves of autoclave after sterilization cycle.

4.5.4.11 Ampoules shall be sampled from all four corners and center of upper, middle and lower shelves to form pool sample for microbiological as well as chemical analysis.
4.5.4.12 After sampling close the containers immediately.
4.5.4.13 Close the sample container/seal the polybag and record the details in BMR and sample request.
4.5.4.14 Send the sample and request for analysis to Quality Control Laboratory for testing.

5.0 REASON FOR REVISION:

This SOP is modified in order to be more effective in its responsibility and procedure.

6.0 TRAINING:
Trainer — Head – Quality Assurance
Trainee — Quality Assurance Officers

7.0 DISTRIBUTION:

Certified Copy No. 1 : Head of Department
Certified Copy No. 3 : Head of Department – Quality Control
Certified Copy No. 4 : Head – Plant Operations
Original Copy : Head – QUALITY ASSURANCE

8.0 ANNEXURES:

Nil.

9.0 REFERENCE:

In-house

 

SOP for testing of ETP water

sop for Calibration and Maintenance of Laboratory Instruments and Equipment

Disposal of Residual Sample or Left Over Material

sop for for Laboratory Incident

standard operating procedure temperature monitoring

sop for drying of silica gel

sop for operation of infrared moisture balance

sop for preparation of mobile phase

sop for treated RO water

sop for Preparation and Issuance of Analysis protocol standard

sop of placebo and impurity stock solutions

sop for disposal of residual sample  

sop for handling of pharmacopoeial changes

sop for procedure for operation of ultrasonic cleaner

difference between UPLC and HPLC

sop for for Emergency Eyewash and Shower

sop for operation and calibration of total organic carbon analyzers

sop for operation of cobb tester

sop for Operation and calibration of atomic absorption spectrophotometer

sop for Operation and calibration of gas liquid chromatograph

sop for operation of humidity oven

sop for operation and calibration of serological water bath

sop for monitoring of drain trap

sop for destruction of analytical samples after testing and control samples

sop for destruction of used chemicals

Sop for Operation of suction pump

sop for Operation and calibration uv cabinet

sop for Operation and calibration of bulk density apparatus

sop for operation and calibration of shore hardness tester

sop for operation of rub proofness tester

sop for monitoring of purified water

sop for Retesting of packaging materials

sop for Retesting and resampling of raw materials

sop for Control of issuance of record of analysis green sheets

sop for Control of computer passwords

sop for sampling of packaging materials PM

sop for sampling of sterile raw material

sop for sampling of intermediates and finished products

sop for operation and calibration of friability test apparatus

sop for approval and rejection of packaging materials

sop for non conformance of RM PM and finished product

sop for collection storage and disposal of control samples

sop for trend analysis of finished products

sop for Chromatographic practices and system suitability

SOP For Good Laboratory Practices

sop for cleaning and operation of sieve shaker

general specification of packing material cartons

sop for Password for Analytical Instrument and LIMS software

sop for Rounding off numerical analytical results

sop for sampling of bulk and finished product

sop for cleaning of spillage material

sop for Handling of Reference Standard

sop for hplc column maintenance and washing

procedure for sampling and handling of bulk sample

STP for borewell generation point (raw water storage tank)

sop for preparation and standardization of 0.1M Zinc Sulphate

Operation &calibration of analytical balance (dhona)

Operation and Calibration Procedure for Disintegration Test apparatus

sop for preparation and standardization of 1 M Hydrochloric Acid

Preparation and standardization of 0.1 M ceric ammonium sulphate solution

sop for preparation and standardization of 0.05 m iodine solution

validation of volumetric solution 0.1m ammonium thiocyanate

handling of reference standard and preparation of working standard

sop for water sampling and analysis

sop for operation for validation of excel worksheets

sop for laboratory cleaning

sop for stability of volumetric solutions

sop for preparation of raw material in process finish product packing material data sheets

sop for handling of hazardous chemicals

sop for handling of glassware and allocation of identification number

sop for operation cleaning and calibration of bursting strength tester

sop for rounding off the analytical test results

procedure for Analyst Qualification

sop for operation and calibration of dissolution Apparatus

procedure for maintenance of desiccators

sop for for hplc column receipt checking id no and regeneration

safety data sheet for laboratory chemicals

procedure for handling of poisonous chemicals

sop for cleaning of sampling devices

sop for calibration procedure of instruments

sop for specification and standard testing raw material packing material and finished product

procedure for operation and calibration of potentiometric titrator

procedure for operating and calibration of digital hardness tester

procedure for disposal of expired chemicals, reagents and solvents

sop for behavior in quality control department

sop for preparation and standardization 0.1M sodium thiosulphate

sop for preparation and standardization 0.1M Disodium Edetate

preparation and standardization 0.1M Sodium Hydroxide Solution

Preparation and standardization of 0.1M Perchloric acid solution

sop for preparation 0.05M edetate disodium

sop for preparation 0.1M silver nitrate

sop for Operation and Calibration of High Performance Liquid Chromatography

sop for UV & Visible Spectrophotometer

procedure for Cleaning of laboratory glassware

Cleaning of Instrument, Instrument bench and surrounding area of Quality

Safety Precaution in Quality Control Department

Operation & Calibration of Analytical Balance

Calibration of Glassware in Quality Control Department

handling of samples received in Quality Control

Cleaning and Operation of Refrigerator

Operation, Cleaning and Calibration of water bath

Operation & Calibration of Refractometer

Operation and Cleaning of Centrifuge Apparatus

cleaning, operation & calibration of Vernier caliper

Calibration of Fourier Transform Infrared Spectrophotometer (FTIR)

Cleaning and operation of Moisture Analyzer

Cleaning & Operation of Vacuum pump in Quality Control Department

Operation and Calibration of Polarimeter

Cleaning and operation of Magnetic Stirrer

Cleaning Operation and Calibration of Melting Point

Operation Cleaning and Calibration of Muffle Furnance in Quality Control Department

procedure of operation and Cleaning of Sonicator

Operation Cleaning & Calibration of pH meter in Quality Control Department

Entry and Exit in Quality Control Department

Exit mobile version