SOP for Sampling and Analysis of Wash Water from Production Equipment

Purpose

The purpose of this SOP is to define the Sampling and analytical procedure for wash water.

Scope

This procedure is applicable for a sampling of wash water from production equipment and analysis of wash water in the Quality Control laboratory of PharmaInfo Ltd.

Responsibility

Production Executive 

• To co-ordinate to collection the sample as per the defined procedure
• To send duly filled Wash Water Sampling Advice Form to QC/QA Department.
• To maintain the proper documentation.

Quality Assurance Executive

• To withdraw the sample as per the defined procedure.

QC Executive

• To analyze the sample as per the defined procedure
• To ensure that this procedure is kept up to date.

Quality Control Manager

• To ensure appropriate personnel from the section are trained on this procedure.
• To confirm that SOP is technically sound and reflects the required working practices.

Head of Quality Assurance

• To ensure the overall implementation of the SOP.
• Approval of the SOP.

Definitions

Procedure ‘A’:

• Cleaning with the help of potable/purified water (Wet Cleaning). Procedure ‘A’ follows every product-to-product changeover and after 5 consecutive batches of the same product, 0.5% SLS shall be used as a cleansing agent in case of water-insoluble product.

Procedure ‘B’:

• Cleaning with the help of a Clean, dry cloth (Dry Cleaning). Procedure ‘B’ follows every batch-to-batch changeover

Procedure

• Production personnel clean the equipment as per standard cleaning procedure and intimates QC/QA for wash water sampling with the “Wash Water Sampling Form” in duplicate.
• Wash water sampling shall be performed after cleaning the equipment for every product-to-product changeover e.g. after cleaning of Procedure ‘A’ and after 5 consecutive batches of the same product.
• Officer / Executive- IPQA shall receive a request for Sampling / Analysis of Wash Water of equipment used in the production department.
• Officer / Executive-IPQA shall collect the wash water sample in a clean, dry amber colour sampling bottle and label the bottle, duly filled and signed.
• Sample for the microbial analysis shall be taken by a Microbiologist in a sterile, clean glass bottle.
• Submit the sample to the QC department for Wash Water Analysis.
• QC shall analyse the sample, and prepare the analysis report and the same shall be sent to the production department.
• After receiving the wash water analysis report for its compliance, the Production department shall affix a ‘CLEANED’ label on the equipment duly filled and signed.

The Quality Control Executive inspects the equipment and its parts for cleanliness and then collects the sample as follows:

Sr. No.	Equipment	Sample Size	Procedure Of Sampling
1	Mass Mixer	30 ml	Add approximately 15 litres of purified water for the final rinsing of the mass mixer, do the mixing for 5 minutes, tilt the mass mixer and then collect the sample in a previously cleaned glass bottle.
2	Rapid Mixer Granulator	30 ml	Rinse the equipment bowl and top lid with 30.0L of Purified water and collect the water into a clean bowl through the discharge taking care that the whole surface of the bowl and top lid is rinsed properly and rinse the dismantled parts (clamp for binder addition, charging port, spray nozzle, vent filter, chopper blade, impeller blade discharge valve and all gaskets) with 5 litres of purified water and collect into the same bowl.
3	Multimill	30 ml	Add 5.0 litre of purified water from the hopper and collect the sample in a previously cleaned glass bottle from an outlet of S.S. cover of the multimill.
4	Comminuting mill (Cadmill Or Clitmill)	30 ml	Add 5.0 litre of purified water from the hopper covering the whole surface area and then collect the sample in a previously cleaned glass bottle from an outlet of the cadmill.
5	Fluid Bed Dryer	30 ml	Rinse the retarding chamber internally with 10.0 L of Purified water and collect it into a clean bowl. Similarly, rinse the FBD trolleys with 10.0 L of Purified water each and collect 30ml of the sample separately from the two bowls. Rinse the cartridge filters/FBD bag with 5 litres of purified water and collect the water into the clean bowl.
6	Container Blender		Rinse the colloid mill with 3.0 L of Purified water and collect it into a clean bowl.
7	Bin Blender Capacity: 1200 L 800 L 400 L 200 L 50 L	30 ml	Add 20.0 litre of purified water into the bin blender and after closing rotate the blender for 5 minutes, open it and then collect the sample in a previously cleaned glass bottle. Add 15.0 litre of purified water into the bin blender and after closing rotate the blender for 5 minutes, open it and then collect the sample in a previously cleaned glass bottle. Add 10.0 litre of purified water into the bin blender and after closing rotate the blender for 5 minutes, open it and then collect the sample in a previously cleaned glass bottle. Add 5.0 litre purified water into the bin blender and after closing rotate the blender for 5 minutes, open it and then collect the sample in a previously cleaned glass bottle. Add 4.0 litre purified water into the bin blender and after closing rotate the blender for 5 minutes, open it and then collect the sample in a previously cleaned glass bottle.

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8	Vibratory Shifter	30 ml	Attach the sieve to the body of the sifter wash with 3.0 L of Purified water and collect the sample at the receiver into a clean bowl. Rinse the dismantled parts (Lid, clamp, hopper and silicon gasket) with 2 litres of purified water and collect them into the same bowl.
9	Compression Machine	30 ml	Rinse the hoppers, butterfly valve, tri-clover clamp, force feeder, inlet connector, Turret guards, Powder scrapper, Acrylic guards, feeder shaft, and Exhaust pipes with 5 litres of purified water and collect in a clean bowl. Collect approximately 30 ml of this sample into an amber-coloured bottle for analysis. Similarly rinse the y – chute, and Gravity pipe with 5 liters of purified water and collect in the clean bowl.
10	Roll Compactor	30 ml	Add 5.0 litre of purified water from the hopper and collect the sample in a previously cleaned glass bottle from an outlet of the bottom end of roll compactor.
11	Tray Dryer	30 ml	Add 500 ml purified water in each tray and spread it covering the whole inner surface area. Collect purified water of all trays in an SS Container, and collect samples in a previously cleaned glass bottle from the container.
12	Double Cone Blender	30 ml	Add 5.0 litre purified water into the Double cone blender and after closing rotate the blender for 5 minutes. Open it and then collect the sample in a previously cleaned glass bottle.
13	Coating Pan	30 ml	Pour 10.0 litre of purified water in the coating pan and run for 5 minutes. Collect sample in previously cleaned glass bottle.
14	Tablet Coating Machine	30 ml	Rinse the pan with 10.0L of Purified water and collect the sample into a clean bowl through the discharge taking care that the whole surface and the Baffles are rinsed properly. Rinse the dismantled parts (Silicon tube, Gun assembly, inlet duct and outlet duct) with 5 liters of purified water and collect into the same bowl.
15	Capsule Filling Machine	30 ml	Rinse the capsule loading channel, hopper, loading ring, Auger, locking pin assembly with 5 liters of purified water and collect in to clean bowl. Collect approximately 30 ml of this sample into an amber-colored bottle for analysis.
16	Capsule Polishing Machine	30 ml	Rinse S.S cover of polishing Machine and polishing brush with 2 liters of purified water and collect in a clean bowl.

17	S.S. Items S.S. Tanks and Stirrer	30 ml	Keep S.S. items in S.S. Tub, add 5.0 litres of purified water, collect sample from the tub.
18	Colloid Mill	30 ml	Close the outlet valve, add 2.0 litres of purified water, run the Colloid Mill for 5 to 7 minutes. Open the outlet valve and collect the sample.
19	Jacketed Mixer Cum Homogenizer	30 ml	Rinse volume is 5.0 litres of purified water
20	Storage Container For Gel/ Ointment	30 ml	Rinse volume is 10.0 litres of purified water
21	Pulveriser	30 ml	Rinse volume is 2.0 litres of purified water
22	Filter Press	30 ml	Rinse volume is 20.0 litres of purified water
23	Four (04) Head Rotary Filling M/C	30 ml	Rinse volume is 20.0 litres of purified water
24	Transfer Pumps and Pipes	30 ml	Rinse volume is 10.0 litres of purified water
25	Clitmill	30 ml	Rinse volume is 5.0 litres of purified water
26	Centrifuges Hydroextractor	30 ml	Rinse volume is 5.0 litres of purified water
27	Fabrica Four (04) Head Filling M/C	30 ml	Rinse volume is 2.0 litres of purified water
28	RMG – II	30 ml	Rinse volume is 10.0 litres of purified water
29	RMG – I	30 ml	Rinse volume is 15.0 litres of purified water
30	FBD Bowl – I	30 ml	Rinse volume is 10.0 litres of purified water
31	FBD Bowl – II	30 ml	Rinse volume is 10.0 litres of purified water
32	Sifter Cum Multi Mill	30 ml	Rinse volume is 10.0 litres of purified water
33	Tipper	30 ml	Rinse volume is 10.0 litres of purified water
34	Sifter	30 ml	Rinse volume is 5.0 litres of purified water
35	Starch Kettle	30 ml	The rinse volume is 5.0 litres of purified water
36	Neo Cota	30 ml	The rinse volume is 10.0 litres of purified water
37	Sejong Compression Machine	30 ml	The rinse volume is 5.0 litres of each of purified water from a chute, hopper and other parts
38	Cadpress Compression Machine	30 ml	The rinse volume is 5.0 litres of each of purified water from a chute, hopper and other parts
39	RMG	30 ml	The rinse volume is 5.0 litres of purified water
40	FBD Bowl	30 ml	The rinse volume is 4.0 litres of purified water
41	Kenwood Mixer	30 ml	The rinse volume is 1.0 litres of purified water
42	Hand Filling Machine	30 ml	The rinse volume is 5.0 litres of purified water

Blank Sample:

While collecting the wash water sample, collect Purified water about 30 ml into an amber-colored bottle.

Analysis:

• After getting the sampling advice form from the production department, QC personnel will enter in the wash water register and assign a lab control number as WW-000X/MM/XX

Where,

WW for Wash Water, 

000X- Sequential number of four digits, 

MM-Month

YY-Last two digits of year. 

For example: WW-0001/08/XX). Then the compliance personnel will collect the sample and send to the Quality Control department for analysis.

• QC analyses the sample by scanning through 190-400 nm on UV-VIS Spectrophotometer, using Purified water (collected as explained earlier) as blank.
• Observe for any abnormal peaks and/or peaks having same wavelength maximum of the active material of the previous product.
• Reject the sample in case of any abnormal peak or if a peak of the previous product has more absorbance than that of a 10 ppm standard solution of active of the previous product and send the information to the concerned department.
• Take the spectrum printout on the back side of the wash water report copy (QC copy) and inform production for rewash.
• If absorbance is less than that observed in the standard graph, intimate the concerned department by sending the original copy of the report after making necessary entries and approving the clean card. Retain the duplicate copy of the report and file it after making the necessary entries in the register.

Annexure

Annexure-I: Wash Water Sampling Advice Form.

Annexure-II: Wash Water Register.

Abbreviations

BMR – Batch Manufacturing Record

IPQA – In-process Quality Assurance

SOP – Standard Operating Procedure

QA – Quality Assurance

QC – Quality Control

SS – Stainless Steel

Revision History

Nil

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