Month: March 2021

Preventive Maintenance of Dissolution Test Apparatus


  1. Objective
  1. 1 To describe the procedure for preventive maintenance of Tablet Dissolution Apparatus
  • 2.0 Responsibility
  • Executive  – Quality Control   – To perform the preventive maintenance activity
  • Head – Quality Control            — To ensure compliance against established schedule
  • 3.0 PROCEDURE
  • 3.1 Precautions:
  • 3.2 Ensure that the power supply to the instrument is switched “off” before starting the preventive maintenance.
  • 3.3 Clean the instrument with a clean dry cloth every day.
  • 3.4 Performance checks shall be done for the following parameters as per SOP no. QC070 before performing preventive maintenance.
  • Vessel temperature
  • RPM
  • Paddle/Basket Height
  • Timer
  • Wobbling of paddle/basket
  • Eccentricity
  • 3.5 Enter the values in standard maintenance card as per SOP preventive maintenance procedure for laboratory instruments
  • 3.6 The following components of the dissolution shall be subjected for preventive maintenance on the schedule date.
  • 3.7 DISSOLUTION BATH:
  • Remove the heater connections from the control panel
  • Check for leaks/cracks outside the bath after filling with fresh purified water.
  • Jar holder connections shall be verified, replace in case of  any damages.
  • Remove the water from the bath and clean the heater with smooth dry cloth, replace in case of any scratches found on heater.
  • Temperature sensor shall be cleaned with smooth polished cloth.
  • Heater connects shall be verified.
  • 3.8 SYSTEM CONTROLLER:
  • Remove the cover of the system controller, clean inside portion with a smooth nylon brush.
  • Check the spindle belts and carrier bearings, replace new belts or bearings in case of any discrepancies.
  • Spindle stepper motor shall be verified and cleaned with smooth brush.
  • Check electronic circuit with a multimeter and repair the respective affected circuits.
  •  Circuit-cooling fan shall be verified for properly functioning.
  •  Clean the motor with smooth brush.
  • Spindle bearings shall be verified for any corrosion, replace when any bearing   got corrosion.
  • 3.9 BODY OF THE DISSOLUTION APPARATUS:
  • Check for any abnormal sound is observed at lifting bearings
  • Apply the grease to lifting bearings.
  • Apply engine oil to lift road at backside.
  • Lift motor condition shall be checked and repaired.

          Frequency of the Preventive maintenance for Dissolution Apparatus is once in 3  months.

  • 4.0 ABBREVIATIONS
  • SOP – Standard operating procedure
  • PM – Preventive maintenance
  • QC- Quality Control
  • 5.0 REFERENCE
  • Sop – calibration of dissolution apparatus
  • Sop preventive maintenance procedure for laboratory instruments
  • 6.0 ANNEXURES

Nil

Preventive Maintenance of HPLC’s


  1. OBJECTIVE:

1.1        To describe the procedure for preventive maintenance of HPLC’s

2. RESPONSIBILITY:

2.1       Executive  – Quality Control– To perform the preventive maintenance activity.

2.2        Head – Quality Control  – To ensure compliance against established schedule.

3. PROCEDURE

      Precautions:

3.1       Ensure that the power supply to the instrument is switched “off” before starting the preventive maintenance.

3.2       Clean the instrument with a clean dry cloth every day.

3.3       Performance checks shall be done for the following parameters as per Calibration sop After doing preventive maintenance

3.4       Enter the values in standard maintenance card as per sop Preventive Maintenance procedure for Laboratory Instruments.

3.5       The following components of HPLC shall be subjected for preventive maintenance on the schedule date.

3.5.1 Pump Solvent Separation Module

3.5.1.1  Switch off the main power switch provided on the backside.

 3.5.1.2  Clean front panel and cover

3.5.1.3 Sonicate solvent inlet filters, drain valve filter inlet and outlet check  valves in methanol for 5 min.

3.5.1.4 open pump head check plunger and plunger seal for scratches on the   plunger, replace if necessary

3.5.1.5 Check seal wash assembly seals, replace if necessary.

3.5.1.6 Check and sonicate inlet valve cartridges

  3.5.1.7 Check pump functioning for pressure fluctuations.

  3.6    Auto Injector

           3.6.1    Check the injector syringe, replace if necessary

          3.6.2    Clean all tubes in injector

          3.6.3    Perform the purge and compression ensures all fitting are tight.

         3.6.4    Adjust seal pack if necessary to optimise the needle port.

        3.6.5    Check needle and the seal pack seals replace if necessary.

  3.7    Column Oven

            3.7.1     Remove dirt from panel and cover

            3.7.2     Check the function of circuit cooling fan, replace if it is not working.

           3.7.3     Check column oven functioning

          3.7.4     Check leak sensor functioning

  • 3.7.5 Check tubing connections for damages, cut tubing and replace new tubing if 

             Necessary.

   3.8  Detector

          3.8.1   Check the intensity and running hours of  lamp, replace if necessary.

         3.8.2  Remove the flow cell and sonicate it for 10 minutes in methanol with water. 

         3.8.3    Fix the flow cell back after sonication.

        3.8.4    Purge the detector with methanol and nitrogen.

  • 3.9 Enter the preventive maintenance checks in standard maintenance card as per   
  • 3.10 Stick the under preventive maintenance label before doing preventive maintenance as per SOP  

             Preventive Maintenance procedure for Laboratory Instruments.

3.11  Stick the preventive maintenance status label duly filled as per SOP Preventive Maintenance procedure for Laboratory Instruments.

3.12      Frequency of schedule is every 3 months.

4.    ABBREVATIONS

     4.1       SOP – Standard Operating Procedure

      4.2       HPLC – High performance liquid chromatography

4.3 QC-Quality Control.

5.   REFERENCES

      5.1       SOP Preventive Maintenance procedure for Laboratory Instruments.

6.    ANNEXURES

      Nil.

Qualification of Analyst in Quality Control


  1. OBJECTIVE

1.1 To lay down a procedure for  training and a mechanism to evaluate a chemist on General Analytical techniques.

2.          RESPONSIBILITY

2.1        Personnel who are knowledgeable with the subject virtue of their qualification and   experience, to train the analyst as required.

  • Head – Quality Control – To ensure the compliance of SOP.
  •  PROCEDURE
  • All the analyst undertaking any analysis shall undergo training and qualify on relevant Standard Operating Procedures (SOPs), and General analytical techniques. The general analytical techniques along with acceptance criteria on which the analyst are to be trained are listed in Annexure – 1.
  • The training on analytical techniques shall be carried out under the supervision of the senior executive or a analyst already trained on that technique, by following the Standard Test Procedure / Standard Operating Procedure and using already approved product / material as test sample.
  • To qualify on the analytical technique the analyst shall perform the test. The results shall   be comparable with the results already reported and meet the acceptance criteria as given in Annexure – 1.
  • All the analytical data with calculations to be entered in the work sheet as Annexure-2 all back up date like chromatograms, balance print outs to be enclosed with work sheet only
  • QC In charge / His Designee shall review and evaluate the data generated by the analyst. If the results are satisfactory as mentioned above, it can be concluded that the analyst is qualified to perform the particular technique. In case of any discrepancy or abnormality observed, it can be investigated, counseled and by omitting the mistakes, if any training shall be repeated and again evaluated.
  • Lectures on technical subjects shall be conducted by qualified in-house / external staff.
  • Evaluation of training shall be done by conducting oral / written tests, demonstrations and presentations.
  • Apart from the technical training related to Quality Control operation, all additional training is outlined in the SOP “TRAINING OF PERSONAL” SOP No. XYZ by QA department.

4.         ABBREVIATIONS

4.1       QC     –    Quality Control

4.2       QA     –    Quality Assurance

4.3       SOP   –    Standard Operating Procedure

4.4       STP   –    Standard Testing Procedure

5.         REFERENCES

  • “TRAINING OF PERSONAL IN THE FACTORY”

6. ANNEXURES

6.1      Annexure – 1     Acceptance criteria for qualification of the analyst.

6.2      Annexure – 2     Work sheet

ANNEXURE-1

ACCEPTANCE CRITERIA FOR QUALIFICATION OF ANALYST

S. No.Analytical TechniqueGeneral Procedure for TrainingAcceptance criteria
1.Assay by HPLCThe analyst shall perform the assay five times (five replicate sample preparation).1.The System suitability requirements, if any shall pass. 2.The RSD of five replicate assay values shall be NMT 1%.
2.Dissolution by UVThe analyst shall perform the dissolution of 6 tablets/capsules approved by following the STP and GTP.1.The System suitability requirements, if any shall pass. The RSD for 6 tablets dissolution shall be NMT 5%
3.Residual Solvents/OVI by GCThe analyst shall perform the test in duplicate (two replicate sample preparations).1.The System suitability requirements, if any shall pass. 2.The duplicate values shall be within ± 20% from the average values.
4.Assay by titrimetry/ PotentiometryThe analyst shall perform the assay five times (five replicate sample preparations).1.The RSD of five replicate assay values shall be NMT 1%.
5.LOD/Water by KFThe analyst shall perform the test five times (five replicate sample preparations).1.The RSD of five replicate LOD values shall be NMT 10%. The individual values of water by KF shall be within ± 0.2% from the average value.
6.TLC (for related substances limit tests/identification)The analyst shall perform the test in duplicate (two replicate sample preparations).The System suitability requirements, if any shall pass. The intensity of spots and corresponding Rf values shall match in duplicate samples.
7.Identification by IRThe analyst shall perform the test in duplicate (two replicate sample preparations).The spectrum of duplicate sample shall show similar pattern as that of the standard.  
S. No.Analytical TechniqueGeneral Procedure for TrainingAcceptance criteria
8.  a) Sulphated ash b)Residue on ignition c)Loss on ignition d) Heavy metals e) Limit test for Arsenic, Iron, lead.The analyst shall perform the test in duplicateDuplicate values shall be within ±0.05% The duplicate solution shall match visually and shall be less than the standard solution.
9.Bulk densityThe analyst shall perform the test in duplicate (two replicate sample preparations).The duplicate values shall match.
10.Distilling range/melting point/melting rangeThe analyst shall perform the test in duplicate.The duplicate values shall match.
11.Powder fineness . particle size analyzer/by Sieve analysisThe analyst shall perform the test in duplicateThe duplicate values shall match.
12.Standardization of volumetric solutionAnalyst shall standardize any volumetric solution  in duplicate.The difference between the duplicate values shall  be not more than 0.2%.
13.ViscosityThe analyst shall perform the test in duplicate (two replicate sample preparations).The duplicate values shall match.
14.Specific rotationThe analyst shall perform the test in duplicate (two replicate sample preparations).The duplicate values shall match.
15.FriabilityThe analyst shall perform the test in duplicate.The duplicate values shall match.
16.DisintegrationThe analyst shall perform the test in duplicateThe duplicate values shall match.
17.Acidity and alkalinity Appearance of solutionThe analyst shall perform the test in duplicate (two replicate sample preparations).The duplicate values shall match.
18.Microbial limit testThe analyst shall perform the test in duplicate (two replicate sample preparations).The duplicate values shall match and should not show different type of colonies.
19.Chlorides SulphatesThe analyst shall perform the test in duplicate (two replicate sample preparations).The duplicate values shall match
20.TOCThe analyst shall perform the cleaning samples in duplicate.The duplicate value shall match.
S. No.Analytical TechniqueGeneral Procedure for TrainingAcceptance criteria
21.Bursting strength testerThe analyst shall perform the test in duplicateThe duplicate value shall match.
22.Thickness testing (by micrometer)The analyst shall perform the test in duplicateThe duplicate value shall match.
23.Dimensions (by scale)The analyst shall perform the test in duplicateThe duplicate value shall match.
24.GSM (grammage)The analyst shall perform the test in duplicateThe duplicate value shall match.
25.GSM of VMCH coatingThe analyst shall perform the test in duplicateThe duplicate value shall match.

ANNEXURE – 2

Worksheet

PRODUCT/ MATERIAL:BATCH No.:ISSUED ON:
SPECIFICATION No.:A.R.No.:COPY No.: 
STP No.:ISSUED BY:PAGE No.:

Procurement, Inspection, Storage, Usage, Polishing and Cleaning of Punches and Dies


 1.0 OBJECTIVE

  • To lay down a procedure for Procurement, Inspection, Storage, Usage, Polishing and Cleaning of Punches and Dies, which are used as tabletting tools.

2.0 RESPONSIBILITY

  • Technical Assistant – To follow the SOP.
  • Executive – To comply the SOP.

3.0 PROCEDURE

3.1 PROCUREMENT OF PUNCHES AND DIES:

  • Production department shall identify the required tabletting tool while reviewing the “DRAFT FOR REVIEW” copy of the particular Batch Processing Record of the particular product.
  • Based on the above requirement the production personnel shall coordinate with FRD for necessary approved design of punches used in the product development of the particular product.
  • Depending upon the approved drawing issued by FRD, the production department shall raise Design Specification (Annexure – 1) for the required sets of tabletting tool.
  • In design specification the production personnel shall give the detailed description of the Upper punches, Lower punches, Dies embossing details with required specifications and if any special recommendations for the supplier.
  • Finally the design specification shall be forwarded to Head – QA for authorization.
  • After the approval of the design specification by Head QA, the production personnel shall raise the indent for punches & dies, 35sets for Sejong 30stn. compression machine and 50sets for 45stn. compression machine.
  • The respective personnel along with the design specification shall approve the indent copy.
  • After the approval of indent copy, Purchase Order shall be raised along with the approved design specification.
  • Based on the above design specification the party shall submit the relevant Inspection Reports, MOC certificates, DQ’s, any aids like GO-NO-GO-Gauge etc.
  • The production personnel shall critically review after receiving the punches and dies, all relevant submitted data thoroughly against the established Approved Design.
  • If everything is satisfactory, the tabletting tools shall be subjected for inspection by production department and cross – checked by Engineering and QA deportment.
  • The inspection details shall be recorded as per Annexure – 2.
  • After completion of inspection, Head – Production, Engineering department and Quality assurance personnel shall critically review the inspection report against the approved design.
  • Any non confirming to the specification will be immediately returned to the suppliers for the replacement. Only inspected and good sets will be kept in change parts room in provided rack (production).
  • The unique no. shall be allotted as the following example:

             Ex: S-001-00

  • The first letter “S” indicates the Set Number.
  • The second letter is “dash”.
  • The next three digits indicate that sequential number of the set of the punches.
  • The last two digits indicate the No. of inspections carried.

3.2 Inspection Procedure

  • Use only the calibrated instruments for measuring the dimensions of the punches and dies.
  • Wipe off the oil from the surface with the lint free cloth and clean the punch and die sets to be inspected. Check all the punches and dies for any wear and tear or damaged surface.
  • Check the body diameter, punch length (overall and working), tip size, cup depth and concentricity for upper and lower punch, die diameter, height and bore.
  • Record the inspection of the punch and die as per the Annexure -2,3,4,5.

The following instruments are to be used to check the dimensions of various tooling as part of routine maintenance procedure:

  • Comparator.
  • Dial gauge.
  • Pointed brass anvil.
  • Ball anvil.
  • Length gauge.
  •  Appropriate punch holder (D Type).
  •  Vertically held V-block used in place of a punch holder.
  •  Micrometer.
  •  Die Bore GO-NO-GO gauge.
  •  Head GO-NO-GO gauge.
  •  Magnifying glass.
  • 3.3 SETTING UP THE COMPARATOR:
  • It is used to measure overall length, working length and tip to barrel concentricity of a punch. An optimal comparator with overlays also is used to check head profiles and overall length. The described steps for setting up the comparator should be followed carefully.

NOTE: The pointed brass anvil is used for punches with embossing or bisects lines and for punches with small tips and deep concavities. The ball anvil is used for flat and plain concave punches.

  • Place the length gauge on the comparator base under the dial indicator anvil while depressing the lifting lever.
  • Move the dial indicator unit on the pillar until it makes contact with the length gauge.
  • Continue to move the indicator until the pointer has made a sufficient revolution of dial to measure the appropriate depth of the punch concavity or barrel. Then send the indicator to zero.

NOTE: The number of revolution of the pointer will be shown on the small insect dial.

  • Remove the length gauge.
  • 3.4 PROCEDURE FOR MEASURING OVERALL LENGTH:
  • Place the punch in holder with tip in recessed end and head pointing up.
  • Place holder on base of comparator, depress lifting lever to raise anvil and slide punch and holder under the anvil.
  • Lower the anvil carefully on the head flap and record the indicator reading.
  • 3.5 PROCEDURE FOR MEASURING WORKING LENGTH:
  • Place punches in holder with head in recessed end and tip pointing up.
  • Place holder on base of the comparator depress lifting lever to raise anvil and slide punch and holder under the anvil.
  • Lower the anvil carefully on to the punch face and find the deepest point moving the punch and holder around until the dial indicator shows the minimum reading.
  • Subtract this minimum reading from the measured overall length and compare the difference to the theoretical or calculated cup depth. If the punch meets the standard, the difference in the length should closely approximate the cup depth.
  • The working length is the most critical punch dimension, because it controls tablet weight and thickness.
  • 3.6 PROCEDURE FOR MEASURING OF CUP DEPTH:
  • Obtain the theoretical depth of the cup from the tooling drawing or calculate the depth using for the formula for cup depths.
  • To find the actual cup depth, subtract the measured working length from the measured overall length.
  • Check the tolerance shown on tooling drawing or relevant tolerance charts to determine the diameter meets specification.  
  • 3.7 PROCEDURE FOR MEASURING TIP TO BARREL CONCENTRICITY:
  • Set up the comparator with a ball anvil and V – block.
  • Place V – block on comparator base, place punch in V block without side edge of the punch tip or tip straight under the indicator anvil to ensure sufficient register on the dial T.I.R.
  • Carefully rotate the punch and note pointer deflection, which should not exceed as per limits.

NOTE: Total indicator reading is the difference between the highest and lowest  readings taken during the rotation on the punch, eccentricity or deviation  from total indicator reading that exceed as per limits is excessive and could be caused by poorly manufactured tools.

  • 3.8 PROCEDURE FOR MEASURING PUNCH BARREL / BODY DIAMETER:
  • Measure barrel diameter with the micrometer.
  • Check the tolerance shown on tooling drawing or relevant tolerance charts, to determine if the diameter meets specification.
  • 3.9 PROCEDURE FOR MEASURING PUNCH TIP DIAMETER:
  • Measure the tip diameter with a micrometer.
  • Check the tolerance shown on tooling drawing or relevant tolerance charts to determine the diameter meets specification.
  • Using radius gauges that are thin steel templates and contain the range of internal and external criteria. Check the radius of punch faces, when the gauge is compared to the punch face there should be a good match of radius.
  • 3.10 PROCEDURE FOR CHECKING PUNCH HEAD AND NECK FACE
  • Using a go-no-go gauge check the punch head first by passing it through the go end, then check the head does not pass through the no go end.
  • Reject the punches not passing through the go end or that passes through no go end.
  • 3.11 PROCEDURE FOR INSPECTING PUNCH TIPS:
  • Use a magnifying glass to inspect the outside of the tip edges.
  • Check tip edges for raised burrs by visually inspecting the tip edge and / or by drawing a fingernail across the tip edge, be careful not to leave finger on the punch.
  • Visually inspect tip straight for scoring.
  • 3.12 PROCEDURE FOR INSPECTING THE PUNCH FACES:
  • Use a magnifying glass to inspect the punch faces for abrasion.
  • Visually inspect punch faces for corrosion.
  • 3.13 PROCEDURE FOR INSPECTING THE PUNCH HEADS:
  • Use magnifying glass.
  • Check under the head for irregular or excessive wear of the inside head angle.
  • Check the top of the head and head flat.
  • 3.14 PROCEDURE FOR DIE INSPECTION:
  • Die height is measured with micrometer. Alternative method is to use a comparator with a ball anvil on the dial indicator.
  • Die outer diameter is measured with micrometer.
  • Round die bores and shaped die bore are measured by passing the bore through go end of the appropriate GO-NO-GO. If the bore is correct size, the go end will pass through the bore whereas no go end will not.
  • 3.15 STORAGE OF PUNCHES:
  • Smear each punch and die with food grade oil (SYNTEL-H-1 grade) before replacing them back in respective boxes and store in the designated racks.
  • Inspection of the punches and dies shall be subjected for re-inspection after every 5 million tablets of compression of each set.
  • In case any deviation observed from the standard specification in the re-inspection, the respective punches shall be subjected for destruction with (As per Ref. SOP No.PR093) with prior approval from Head-Production.
  • The respective destruction details shall be recorded in the remarks column of the respective punch inspection report.
  • 3.16 USAGE OF PUNCHES AND DIES:
  • Technical Assistant should show all the required punches and dies to the Executive-Production before taking it for the compression of the batch.
  • Check all the punches and dies immediately after completion of the batch compression in presence of Executive-Production.
  • The sets shall be issued in a manner such that all the sets (actual qty. required for the machine +NLT 15% extra) on the rotational basis.

Ex :-     For a 30 station machine normally 35 sets are ordered. During routine usage only 30 sets shall be issued. On the 1st issuance set no.s 1 to 30 shall be issued, for the 2 nd 2 to 31, so on & so forth till Sl no.s 6 to 35, next issuance 7 to 1 up to 30 to 25. After sequence shall restart from Sl no.s 1 to 30 & continued in rotational manner.

  • Enter the details in the punch and die usage record as per Annexure-6.  
  • 3.17 POLISHING PROCEDURE OF PUNCHES AND DIES:
  • Use buffing machine for polishing of punch and dies.
  • RPM of the machine can be controlled for cleaning and polishing of punch tip and die-bore.
  • Procedure the following tools compounds before polishing.
  • Magnifying glass for identifying the damaged surface and finish of the tip.
  • Nylon brush, (cup type) with emery paste for cleaning and polishing of punch tip.
  • Oilstone and lapping stick for removing the burr or claw.
  • Felt bob, with emery paste for polishing embossed tips.
  • Emery paper or emery flour for removing corrosion from the tools.
  • Nylon brush (wheel type) for polishing embossed tips.
  • Silicon paste or emery flower for improving the surface finish. Finally polishing with diamond past for good surface finish.
  • 3.18 CLEANING PROCEDURE OF PUNCHES AND DIES AFTER POLISHING:
  • After polishing, mop the punches with lint free cloth.
  • Place the punches and dies in a cleaned tray separately.
  • Clean them with Iso Propyl Alcohol by using lint free cloth.
  • Apply Food grade oil in and outer surface of the punches and dies.
  • Keep them in the punch tray.
  • Put the Punch tray in the punch rack cabinet.
  • Clean the area thoroughly.
  • Clean the Polishing kit properly and keep it in its regular position.

NOTE: Punch polishing to be done after compression of 1 million tablets of each punch (Approximately).

SOP for Performing Area Qualification


1.0 OBJECTIVE

To provide the detail procedure for qualification of an area.

2.0 SCOPE

This SOP applies to qualification of all areas which are used for storage and process of material and which may affect the product quality, safety, efficacy and storage.

3.0 RESPONSIBILITY

Officer/designee – QA:  To prepare area qualification protocol and report. To execute qualification in co-ordination with other departments.

Officer /designee of user department shall be responsible for execution of area qualification.

Head of Department (HOD) of user department shall responsible for review of area qualification protocol and report.

Head – QA shall be responsible for approval of area qualification protocol and report.

4.0 PROCEDURE

4.1 Officer/designee – QA shall prepare, HOD of user department shall review and finally Head – QA shall approve.

4.2 Parameters shall be considered for area qualification (but are not limited to):-

Classification of area

Men and material movement

Electrical power point

Earthing

Walls, floor and ceiling

Door interlocks

Luminance in area

Safety devices

Utilities in area

Differential pressure in area

The above parameters shall be selected for area qualification as per designed area.

4.3 Men and material movement verification:

Methodology: Using a prototype movement in an area, verification of men and material movement shall be carried out with reference to the design qualification and documented on area layout.

Acceptance criteria: As per design qualification.

4.4 Electrical power point:

Methodology: All electrical power connection in an area shall be checked by using     multimeter.

Acceptance criteria:

Single phase voltage: 230 V ± 10%. Frequency: 50 Hz ± 5%

Three phase voltage: 415 V ± 10%. Frequency: 50 Hz ± 5%.

4.5 Earthing:

Methodology: Earthing shall be checked by using calibrated multimeter.

Acceptance criteria: Not more than 10 Ω.

4.6 Walls, floor and ceiling:

Methodology: Finishing of the walls, floor and ceiling shall be verified as per the design.

Acceptance criteria: Walls, floor and ceiling shall be smooth, easily cleanable, and free from crevices and damages. All corners shall be rounded to provide easy and effective cleaning.

4.7 Door interlocks:

Methodology: Doors interlock (wherever provided) shall be identified in the general layout of area.

Acceptance criteria: Doors interlock shall be automatic closing systems. Doors shall be smoothly operated.

4.8 Luminance in area:

Methodology: Luminance in an area shall be measured at working height (4-6 feet from the floor). Five readings shall be taken by lux meter from different location as per below illustration.

Acceptance criteria: Not less than 300 lux at working level.

4.9 Sound level in area:

Methodology: Sound level shall be measured at personnel height (4-6 feet from the floor) in an operational area. Five readings shall be taken by Sound Level Meter from different location as per above illustration (point 4.8.1).

Acceptance criteria: Sound level in an area, not more than 80 decibels (dB) at personnel height.

Recommendation: If sound level is observed above 80 dB in an operational area, air muff should put on ears.

4.10 Safety devices:

Methodology: Safety devices/features like Fire extinguisher, Emergency exit door and breakable fire alarm window/ doors etc. shall be identified in the layout.

Acceptance criteria: All the devices should be verified as per the layout.

4.11 Utilities in area:

Methodology: Utility points including drain points in an area shall be checked and identified in the layout.

Acceptance criteria: Utilities like nitrogen gas, steam, potable water, purified water, and compressed air shall be identified in the layout. All the drain points shall also be identified on the plan layout. All drain points shall have water seal.

4.12 Differential pressure in area:

Methodology: Differential pressure (DP) across room/cubicle and corridor, primary corridor and atmosphere shall be recorded shown by magnehelic gauge.

Acceptance criteria:

  • DP across room/cubicle and corridor : between 0.5 – 3.0 mm of wc
  • DP across primary corridor and atmosphere: between 3.5 – 5.5 mm of wc.

4.13 User department shall execute area qualification study as per approved protocol.

4.14 During the execution of protocol, any discrepancy observed shall be recorded and impact assessment carried out as per the respective protocol. After the execution and compilation of protocol, a qualification report is prepared.

4.15 The parameters and acceptance criteria defined herein is for classified areas (ISO class-7 and class-8). For non classified area, depending upon the design qualification, test parameters and acceptance criteria may differ and elaborated in respective protocol.

4.16 Parameters and certificates, if provided by the vendor, the test may not be repeated. Data shall be reviewed and considered, if appropriate.

5.0 RELATED DOCUMENTS

Not applicable.

6.0 REFERENCES

Not applicable.

7.0 RECORDS

Not applicable.

8.0 REVISION RECORD

VersionReason for RevisionEffective Date

Temperature / Relative Humidity Mapping, Re-Mapping and Monitoring


  1. OBJECTIVE:
    • To provide the procedure for performing temperature and/or relative humidity (RH) mapping study.
    • To establish that the temperature and/or relative humidity conditions across the room or area are within the prescribed limits during extreme external weather conditions.
    • To identify the locations where the monitoring sensors should preferentially be located.
  • 2.0 SCOPE:
    • Applicable to (but not limited to) cold storage room, stability chambers, refrigerators, incubators, warehouse(s), in-process material storage areas, manufacturing area, packaging areas, control (reserve) sample storage area at Paithan manufacturing site.
  • 3.0 RESPONSIBILITY:
    • Officer or designee – Maintenance:
      • To prepare, monitor and execute the mapping and re-mapping schedule.
      • To prepare mapping and re-mapping protocol, report and to monitor the activity in co-ordination with external agency.
    • External agency: To perform mapping and re-mapping study.
    • Head – Maintenance or designee, Executive or designee – QA and Head – User department or designee: To review mapping and re-mapping study protocol and report.
    • Head QA: To approve mapping and re-mapping study protocol and report.
    • User department: To monitor temperature or relative humidity in the respective area. 
  • 4.0 PROCEDURE:
    • 4.1 Mapping study:
    • 4.1.1 Officer or designee – Maintenance should prepare the protocol Head – Maintenance or designee, Executive or designee – QA and Head – User department or designee should review the protocol and finally Head – QA shall approve the mapping study protocol .
    • 4.1.2 Officer or designee – Maintenance should prepare the report Head – Maintenance or designee, Executive or designee – QA and Head – User department or designee should review the report and finally Head – QA should approve the mapping study report.
    • 4.1.3 The protocol and report should be numbered as QAVX/MAP/YYY.
  • Where,

QAV: Stands for Quality Assurance Validation

X: Stands for protocol or report. Affix “P” for protocol and “R” for report.

MAP: Stands for mapping.

YYY: Stands for numbering in three digits serially 001, 002, 003……..

  • 4.1.4 For material storage area where temperature control is required, at least 2 (two) mapping study to be performed in order to observe the effect of seasonal variation. That is one during warmest season and one during the coldest season that will establish whether the equipment and devices installed in the area is able to maintain temperature as per the requirement throughout the year even during extreme weather conditions.
  • 4.1.5 For material storage area where temperature and relative humidity is required mapping study to be performed in 3 (three) seasons in order to observe the effect of seasonal variation. That is one during warmest season, one during monsoon season and one during the coldest season that will establish whether the equipment and devices installed in the area is able to maintain temperature and relative humidity throughout the year even during extreme weather conditions.
  • 4.1.6 Seasonal mapping to be performed as per the prevailing condition of the area such as available material, personnel or machinery.
  • 4.1.7 While qualifying storage area, mapping study to be performed considering empty and optimally loaded conditions.
  • 4.1.8 Prior to mapping study, ensure that all the probes or data loggers are within its calibration period. There should be an international recognized standard traceable to 3 point calibration with guaranteed error of not more than ± 0.5°C at each calibration point. Reference of same shall be verified and attached along with the report.
  • 4.1.9 Temperature recording probes should have an accuracy of at least ± 1°C and relative humidity recording probes should have an accuracy of at least ± 3%.
  • 4.1.10 Depending on the size of the area, number of probe or data logger locations and placement shall be determined. Rational for number of probes and its placement to be included in the protocol. Probe placement rational may include (but not limited to):
  • 4.1.10.1 Temperature or relative humidity probes or data logger should be arranged in a grid form along the width and length of the area so that area is reasonably covered with probes or data logger locations every 5 – 10 meters. The selected probe or data logger grid should take account of: 
    • Layout of the area (e.g. whether it is square or includes compartment).
    • The extent to which shelving and products may affect airflow.
    • Suspected cool or warm areas such as near the control sensors and monitoring sensors.
    • If the ceiling height is 3.6 meters or less, arrange probes or data loggers directly above one another at high and low level (e.g. one data logger at floor level, one data logger at 1.2 meters and one data logger at 3.0 meters).
    • If the ceiling height is greater than 3.6 meters, arrange probes or data loggers in vertical arrays at the bottom, middle and top of the space. For storage area of 6 (six) meters in height, 3 (three) probes or data loggers should be placed in each grid location heights of 1.8 meters, 3.6 meters and 5.4 meters.
    • 4.1.11 To eliminate the possible errors and assure consistent execution, following care should be taken.
    • Assign each probes or data logger’s location a unique identification number.
    • Label the exact spot where the data logger should be placed by the sensor’s location name.
    • Create a physical map or photograph with all data logger marked by name.
    • While placing the sensors, consider shelving or pallet racking that may have an effect on the distribution of temperature and humidity and the same to be part of the protocol.   
    • 4.1.12 Areas that are vulnerable for variations in temperature and humidity due to seasonal conditions, mapping study to be carried out for 7 (seven) consecutive days with data recording interval of 15 minutes or below.
    • 4.1.13 For temperature controlled equipment that is not critically affected by seasonal variations in temperature (e.g. Freezer rooms, cold storage rooms, stability chamber and incubator), mapping study should be performed with 24 to 72 hours.
    • 4.1.14 Following information’s (but not limited to) should be part of the mapping study report:
      • Unique ID, make and model no. of the probes or data loggers.
      • Calibration traceability of the probes or data loggers.
      • Graphical data representation.
      • Diagram showing high and low points and point of highest fluctuation.
      • External agency personnel training certificate performing the mapping study.
      • Mean kinetic temperature (MKT) can be applied to each of the separate area being monitored.
    • 4.1.15 Officer or designee – Maintenance shall prepare the report and compile mapping study results received from external agency.
    • 4.1.16 Based on the data collected during mapping study, appropriate summary and conclusion shall be made in the mapping study report.
  • 4.2 Re-mapping study:
    • For re-mapping study, one protocol for each area should be prepared .
    • Protocol number should be :

QAVP/Re-Map/XXX

Where,

QAVP – Stands for Quality Assurance validation protocol.

Re-Map – Re-mapping        

XXX – stands for serial number for re-mapping study

  • Re-mapping study to be carried out as per the approved protocol.
    • After completion of re-mapping study, report should be prepared for each study .
    • Report number should be:

QAVR/ Re-Map /YYY/YY

Where,

QAVR: Stands for Quality Assurance validation report.

Re-Map – Re-mapping        

XXX – stands for serial number for re-mapping study

YY: Stands for serial number of re-mapping of respective area.

  • Re-mapping study to be carried out in below mentioned cases:
    • Periodic re-mapping as per schedule mentioned in Annex–1 for temperature/relative humidity re-mapping frequency.
    • Significant modifications in area equipment.
  • Re–mapping study to be performed as per the prevailing condition of the area such as available material, personnel or machineries.
    • Re–mapping study to be performed for at least three (3) consecutive days with data recording interval of 15 minutes or below.
    • For material storage area, where temperature is being monitored, re-mapping to be performed in summer season.
    • For material storage area where temperature control is required, re-mapping to be performed in summer season.
    • For material storage area where temperature and relative humidity is required, re-mapping study to be performed in summer and monsoon season.
    • Officer or designee – Maintenance shall prepare and maintain the re-mapping schedule as per frequency for temperature/relative humidity re-mapping frequency.
    • 4.3 If the mapping or re-mapping study indicates undesirable conditions, the same shall be investigated and appropriate corrective measures to be taken as below(but not limited to):
      • Removing product from the area.
      • Changing work practices (such as keeping doors open or closed).
      • Changing racking or shelving configurations to improve air circulation.
      • Changing the location of heating devices.
      • Adding air conditioning systems.
      • Improve ventilation.
      • Installing more or large capacity fans.
      • Adding humidification or de-humidification.
      • Installing an HVAC control system.
      • Up gradation or repairing of system.
    • 4.4 After completion of mapping study and evaluation of data, routine monitoring to be performed from following locations:
      • Locations with maximum temperature and relative humidity.
      • Location with highest fluctuation for temperature and humidity.
      • Highest temperature observed at manufacturing area.
      • Any other location as deemed necessary.
      • For semi finished area, location with maximum temperature and maximum relative humidity shall be considered for monitoring during routine process.
      • If identified worst case location is not feasible (such as center of the room, nearby process equipment), next identified worst case location should be considered with adequate justification for routine monitoring.
    • 4.5 Site QA shall maintain the statement of mapping studies performed for various areas along with its dates in an excel spreadsheet.
    • 4.6      In case temperature and relative humidity goes out of limit during daily monitoring with data logger:
      • Inform to maintenance department for the out of limit condition, by using maintenance breakdown form (Format no. MSP/F/169).
      • If rectification requires more than 8 (eight) hours, inform to user department and QA for impact assessment on stored product/material.
      • Based on conclusion of investigation, further necessary action should initiate.   
      • Record the remark on the respective temperature/relative humidity record.
    • 4.7 In case data logger fails during daily monitoring:
      • Inform to maintenance department by using maintenance breakdown form .
      • User should place the calibrated thermometer / hygrometer at location with maximum temperature and high fluctuation temperature/relative humidity to monitor, till the rectification of data logger problem.
      • Record the temperature /relative humidity thrice in a day (one reading should be between 1200 hrs and 1700 hrs).
      • After rectification of data logger failure, thermometer/hygrometer should be removed.
      • In case, the printout facility is disturb for more than 1(one) hour, user department to inform maintenance department by using maintenance breakdown form .
  • 5.0 RELATED DOCUMENTS
  • Nil.
  • 6.0 REFERENCES
    • Temperature mapping of storage areas (Technical supplement to WHO Technical Report Series No. 961, 2011), January 2014
  • 7.0 RECORDS
  • Schedule for temperature/relative humidity mapping study.
    • Temperature/Relative humidity Mapping Protocol.
    • Temperature/Relative humidity Mapping Report.
    • Temperature/Relative humidity Re-mapping Protocol.
    • Temperature/Relative humidity Re-mapping Report.
  • 8.0 REVISION RECORD
VersionReason for RevisionEffective Date
00New SOP 

Installation, Operational and Performance Qualification Report of Vacuum Tray Dryer (VTD)


  Equipment Name :Vacuum Tray Dryer
Equipment Model No.:XYZ
Equipment Sr. No.:XYZ
Equipment ID No.:VTD/XYZ
Equipment Area :Drying room
Equipment Manufacturer Name :
Equipment Application :For drying of wet granules and pellets
Report Date : 

REPORT APPROVAL:         

 Prepared byChecked byApproved by
Signature       
Date     
Name     
DepartmentMaintenanceQuality AssuranceProductionHead -MaintenanceHead – Quality Assurance
Corporate Office: –                                                                                XYZ Factory:-    
Sr. No.TitlePage No.
 Report approval ………………………………………………………1
 Table of contents ………………………………………………………2
 Abbreviations……………………………………………………………3
 Objective ………………………………………………………………4
 Scope …………………………………………………………………4
 Responsibilities …………………………………………………………4
 Equipment description …………………………………………………4
 Procedure ………………………………………………………………4
 Installation verification report …………………………………………4 – 5
 Technical specification verification report ……………………………6 – 8
 Sub components specification verification report ……………………8 – 9
 Measuring Device Calibration Verification Report……………………10
 Utility verification report…….…………………………………………10
 Safety features verification report ……………………………………10 – 11
 Material of construction (MOC) verification report ………………….11 – 12
 Test /inspection certificate verification report ……………………….12 – 13
 Operational functionality verification Report…………………………13 – 14
 Temperature verification report………………………………………15 – 16
 Performance verification report………………………………………16 – 17
 Deviation report ………………………………………………………18
 Change control………………………………………………………18
 List of annexure ……………………………………………………….18
 Summary and conclusion of qualification………………………………19
 Certification of qualification……………………………………………19

Abbreviations: 

Sr. No.AbbreviationFull Form
 °CDegree centigrade
 %Percentage
 ±Plus minus
 ACAlternative current
 cm2Square centimetre
 Dist.District
 DQDesign qualification
 HHeight
 HzHertz
 IDIdentification
 i.e.That is
 IQInstallation qualification
 kgKilogram
 LLength
 MIDCMaharashtra state industrial development corporation
 MOCMaterial of construction
 No.Number
 OQOperational qualification
 PQPerformance qualification
 PRProduction
 QAQuality assurance
 Qty.Quantity
 Sr.Serial
 SSStainless steel
 VVoltage
 VTDVacuum tray dryer
 WWidth
  1. OBJECTIVE:
    1. To record the findings of installation, operational and performance qualification of vacuum tray dryer having ID. No. VTD/XYZ.
2.0        SCOPE:
  • The scope of this report is limited to vacuum tray dryer having ID. No. P/PR/VTD/001.
  • 3.0 RESPONSIBILITIES:
    • Maintenance Officer/Executive:To prepare qualification report and co-ordinate the entire qualification activity.
    • Quality Assurance Officer/Executive: To witness the qualification study and ascertain that the study is conducted as per the protocol.
    • Production Officer/Executive: To execute qualification study in co-ordination with other departments.
    • Head Maintenance: To review the qualification documents.
    • Head Quality Assurance: To review and approve the qualification documents.
  • 4.0 EQUIPMENT DESCRIPTION:
    • AS per installation qualification protocol No.: XYZ/IQ/OQ/PQ/XYZ.
  • 5.0 PROCEDURE:

Qualification of the equipment should meet the acceptance criteria outlined in the following steps.

  • 5.1 Installation Verification Report
Sr. No.Check pointAcceptance Criteria (Specification)ObservationsChecked by Sign/Date
 1.0Visual inspection of the equipment. Visually there should not be any abnormality.  
 2.0Check the area of installation (Dryer area cubicle).Area of installation should have sufficient space for operation and servicing of the equipment.  
 3.0Check the levelling of the machine using level indicator.Air bubble shall be at centre position of level indicator.  
 4.0Check the major components and their electrical cables for housing and anchoring.Major components and their electrical cables shall be securely housed and anchored.  
 5.0Check the electrical ports.     All electrical ports shall be cleaned.  
 6.0Check the electrical circuit diagram.                                                                   All electrical connections shall be found connected as per electrical circuit drawing (reference No. DW-CE010)  
  • Technical Specification Verification Report
Sr. No.Check pointAcceptance Criteria (Specification)ObservationsChecked by Sign/Date
 1.0Loading capacity96 trays with approx 2 – 3 kg material in each trays  
 2.0DimensionApproximate 2750 (L) x 1900 (W) x 2400 (H) mm  
 3.0Heating shelfsHeating shelf’s shall be provided for holding and heating the trays.Sufficient distance shall be provided between two trays after mounting the trays on the shelfs.  
 4.0Door boltsDoor bolts shall be provided to lock the vacuum chamber door.  
 5.0Vacuum pumpVacuum pump facility shall be provided to generate the vacuum in the chamber.  
 6.0CondenserCondenser facility shall be provided for condensing the vapors drawn from vacuum chamber.  
 7.0ReceiverReceiver shall be provided to collect the condensate solvent and to draw vapour through vacuum pump.  
 8.0Digital temperature indicator cum controllerDigital temperature indicator cum controller shall be provided to control the incoming hot water temperature.  
 9.0Digital temperature indicatorDigital temperature indicator shall be provided to display the inlet temperature and product temperature of dryer.  
 10.0Circulation pumpCirculation pump shall be provided to circulate the hot water through drying equipment and tank.  
 11.0Vacuum break valveVacuum break valve shall be provided in front of equipment for easy access.  
 12.0Nitrogen purging valveNitrogen purging valve shall be provided in front of equipment for easy access.  
 13.0View glassView glass shall be provided in front of equipment to view the indoor material.  
 14.0Driving/electrical parts
 14.1Driving and electrical partsDriving and electrical parts shall be covered with SS304 material.There shall be separate cabinet for electrical parts to avoid pollutions from driving parts.  
 15.0Operating panel
 15.1Operating panelOperating panel shall be installed in front of equipment for easy access.  
15.2Emergency stop buttonEmergency stop button shall be provided on operating panel to stop the equipment in emergency.  
  • Sub Components Specification Verification Report
Sr. No.Check pointAcceptance Criteria (Specification)ObservationsChecked by Sign/Date
 1.0CondenserQty.: 1 No.  
 2.0ReceiverQty.: 1 No.  
 3.0Vacuum pumpQty.: 1 Set.  
 4.0Circulation pumpQty.: 1 Set.  
 5.0MotorQty.: 1 No.  
 6.0Sensor details
 6.1Incoming hot water temperature sensorQty.: 1 No.  
 6.2Inlet temperature sensorQty.: 1 No.  
 6.3Product temperature sensorQty.: 1 No.  
 7.0Electrical parts
 7.1Rupture disc/ Explosion ventQty.: 1 No.  
 8.0Pneumatic parts
 8.1Inlet control solenoid valveQty.: 1 Set  
 8.2Steam inlet control valveQty.: 1 Set  
 8.3Vacuum gaugeQty.: 1 Set  
  • 5.3 Measuring Device Calibration Verification Report
Sr. No.Measuring DeviceAcceptance CriteriaID. No./ Sr. No.Calibration  Done On and Calibration Due DateObservationChecked by Sign/Date
 MultimeterIt shall be within its calibration period.    
  • 5.4 Utility Verification Report
Sr. No.Utility parameterAcceptance Criteria (Specification)ObservationsChecked by Sign/Date
 1.0ElectricalThree phase 415 V AC ± 10% and 50 Hz ± 5%.  
 2.0Steam supplyNLT 6.0 kg/cm2  
  • 5.5 Safety Features Verification Report
Sr. No.Safety featuresAcceptance Criteria (Specification)ObservationsChecked by Sign/Date
 1.0EdgesEdges of construction shall be rounded.     
 2.0ElectricityThe equipment shall be earthed.  
 3.0Driving partDriving part shall be covered.  
 4.0Emergency stop buttonEmergency stop switch shall be provided.  
 5.0Sealing systemThe equipment shall consist of inflatable gaskets.  
 6.0Vacuum relief plate/explosion diskRupture disc provision shall be provided to opens at a pressure of 0.25 bar.  
 7.0Control panelControl panel shall be flameproof.  
  • 5.6 Material of Construction (MOC) Verification Report
Sr. No.ComponentAcceptance Criteria (Specification) for MOCObservationsChecked by Sign/Date
 1.0ChamberSS 316  
 2.0TraySS 316  
 3.0Heating shelfsSS 316  
 4.0CondenserSS 316  
 5.0ReceiverSS 316  
 6.0Support columns/legsSS 304  
 7.0Hot water distribution headersSS 304  
 8.0TankSS 304  
 9.0Steam inlet control valveSS 304  
 10.0Silicone rubber gasketsFood grade  
  • 5.7 Test/Inspection Certificate Verification Report
Sr. No.Check pointAcceptance Criteria (Specification)ObservationsChecked by Sign/Date
 1.0MotorIt shall be tested/inspected for its performance.  
 2.0Vacuum pumpIt shall be tested/inspected for its performance.  
 3.0Circulation pumpIt shall be tested/inspected for its performance.  
 4.0SensorIt shall be tested/inspected for its performance.  
 5.0Vacuum gaugeIt shall be tested/inspected for its performance.  
 6.0Control panel flame proofIt shall be tested/inspected for its performance.  
 7.0Rupture discIt shall be tested/inspected for its performance.  
 8.0Steam inlet control valveIt shall be tested/inspected for its performance.  
 9.0Wall panel insulation materialIt shall be tested/inspected for its performance.  
 10.0Vacuum tray dryerGuarantee/Warrantee certificate shall be provided.  

Note: Whether component is tested /inspected of its performance shall be verified based on the test/inspection certificate provided by the manufacturer.

  • 5.8 Operational Functionality Verification Report
Sr. No.OperationAcceptance CriteriaObservationsChecked by Sign/Date
 1.0Turn the main switch panel (red) ON/OFF button to ON position.Main panel shall turn ON.  
 2.0Turn the main switch panel (red) ON/OFF button to OFF position.Main panel shall turn OFF.  
 3.0Press (green) ON button of hot water pumpHot water pump shall turn ON.  
 4.0Press (red) OFF button of hot water pumpHot water pump shall turn OFF.  
 5.0Press (green) ON button of vacuum pumpVacuum pump shall turn ON.  
 6.0Press (red) OFF button of hot water pumpVacuum pump shall turn OFF.  
 7.0By pressing temp set (green) button set the hot water temperature at 90°C.Hot water temperature shall be entered successfully.  
 8.0By pressing up (green) button increase the set hot water temperature.Set hot water temperature shall increase successfully.  
 9.0By pressing down (green) button decrease the set hot water temperature.Set hot water temperature shall decrease successfully.  
  • 5.9 Temperature Verification Report
Sr. No.OperationAcceptance CriteriaObservationsChecked by Sign/Date
 1.0Set the hot water system temperature at 40°C and record the hot water inlet temperature and product temperature from temperature controller panel.For information only  
 2.0Set the hot water system temperature at 50°C and record the hot water inlet temperature and product temperature from temperature controller panel.For information only  
 3.0Set the hot water system temperature at 60°C and record the hot water inlet temperature and product temperature from temperature controller panel.For information only  
 4.0Set the hot water system temperature at 70°C and record the hot water inlet temperature and product temperature from temperature controller panel.For information only  
 5.0Set the hot water system temperature at 80°C and record the hot water inlet temperature and product temperature from temperature controller panel.For information only  
 6.0Set the hot water system temperature at 90°C and record the hot water inlet temperature and product temperature from temperature controller panel.For information only  
  • 5.10 Performance Verification Report
  • 5.10.1 LOD Report:

Minimum capacity of VTD:

Product Name :Batch No.:
Batch Size :
  Sr. No.Sample LocationLOD Result at InitialLOD Result at EndChecked by sign/date
 1.0Top Centre Tray   
 2.0Middle Centre Tray   
 3.0Bottom Centre Tray   
  • 5.10.2 LOD Report:

Maximum capacity of VTD:


Product Name :
Batch No.:
Batch Size :
  Sr. No.Sample LocationLOD Result at InitialLOD Result at EndChecked by sign/date
 Top Centre Tray   
 Middle Centre Tray   
 Bottom Centre Tray   
  • 5.10.3 Temperature mapping study report:

Temperature mapping study is carried out with maximum batch size (i.e. by loading 96 trays with approximately 2 to 3 kg material in each tray) with data recording interval of 15 min.


Product Name :
Batch No.:
Batch Size :
  • Minimum temperature location:
    • Highest fluctuation location:
    • Maximum temperature location:
  • 6.0 DEVIATION REPORT:
Sr. No.Deviation (s)Justification for acceptance criteriaImpact on installation, operation and performance
            
            
            
  • 7.0 CHANGE CONTROL:
  • 8.0 LIST OF ANNEX:
  • 9.0 SUMMARY AND CONCLUSION OF QUALIFICATION:
  • 10.0 CERTIFICATION OF QUALIFICATION:

Qualification is satisfactory.                                       Yes/No

Hence equipment can be used for routine use.           Yes/No

                                                                                                            Head – QA

Acceptable Quality Level (AQL) in Pharmaceuticals


What is Acceptable Quality Level (AQL) :

Acceptable Quality Level (AQL) is a percent defective that is the base line requirement for the quality of the product. The sampling plan required to be prepared or design in such a way that there is high probability of accepting a lot that has a defect level less than or equal to the AQL.

Background of Acceptable Quality Level (AQL) :

The AQL was popularized by Harold F. Dodge and Harry Remig for US military  during World War II. The military faced a problem with the need to test bullets for quality and function. So the military had find a way to test enough bullets to give them assurance about the quality of a lot without testing all bullets. Sampling with AQL addressed these concerns. By pulling a sample of bullets randomly from a lot, the military was able to test part of the lot and use those results to estimate the quality of the total lot. 

Procedure of AQL :

AQL Shall be performed for Packing material ( Printed cartons, Leaflets, Aluminium Foil, PVC/PVDC, Bottles, Caps etc. and for Empty capsule also before sampling or during sampling. AQL shall be performed at different stages of manufacturing like for Compressed tablet, Filled Capsules and Coated tablets after visual Inspection. Both Production and Quality Assurance shall performed the AQL activity .

After getting satisfactory AQL result tablets or capsules shall be further processed to the next stage.

Samples for AQL Inspection shall be collected from each container of the batch or Box.

For Tablets, Capsules and Caplets etc. the Lot Size is equal to the total No. of Tablets, Capsules and Caplets available in respective container.

To determine the “Code Letter” & “Sample Size” corresponding to the “Lot Size” for AQL inspection refer below table A as Single sampling plan for normal inspection and refer below Table B as Single sampling plan for tightened inspection.

Collect the approximate sample into the separate sample bag with the help of “Code Letter”. Refer the Single sampling plan for Normal inspection (Refer table A) and Single sampling plan for Tightened inspection (Refer Table B).

Acceptable Quality Level (AQL) inspection shall be carried out in the “Inspection area” on the SS tray lined with polythene bag and record the result in Acceptable Quality Level (AQL) Report . Inspection shall be carried out on the basis of Classification of Minor, Major & Critical defects.

The Accepted units shall be kept in respective container and only Rejected units shall be kept separate for reference purpose till decision of release or rejection of the batch. These units shall be kept in secured container.

In case of Major or Minor category if numbers of Rejected units are equal / less than the Acceptable criteria, the respective container(s) are accepted and the lot or batch shall be released for further process.

In case of Major or Minor category, if number of Rejected units are equal / more than the Rejection Criteria, the respective container(s) shall be given for 100 % inspection to remove defective units. In case the Rejection is Critical category, then all containers shall be given for 100 % inspection.

On completion of 100 % inspection, again sampling shall be carried out from respective container(s) or all container(s) and AQL Inspection (Tightened) shall be performed.

In case of failure of AQL, Investigation shall be carried out to find out the root cause of failure .

After completion of AQL Inspection, Acceptable units of sample shall be kept in container & Rejected units of sample shall be destroyed.

AQL Inspection Report shall be attached with Batch Manufacturing Record (BMR).

Sampling plan for Normal inspection (Table A)

Sampling plan for Tightened inspection (Table B)

AC Stands for Accepted and RE Stands for Rejected

AQL Calculation :

Suppose we have to perform AQL for Coated tablet or Filled capsule or Compressed tablets and calculated average weight of tablet or capsule after Inspection is 700 mg and Weight of HDPE drum or container with capsule or tablet is 20.00 kg then the calculation will be as follows.

20 kg/700 mg x 1000 x 1000 = 28571 capsules or tablets in Nos.per container. Refer the Lot size (in Nos) & code letters from Table A and B. Refer Serial number 12 whose lot size is mentioned 10,001 to 35,000 and code letter mentioned M that means we have to collect 378 tablets or capsules from each container or drum to perform AQL and based upon the result we have to released the batch.

What is Critical Defects :

It is one that will affect the quality of the finished product (unsafe) and cause a potential risk to the patient. The AQL for critical defects is very low i.e. 0.0%.

What is Major Defects :

It is one that will likely to cause non-conformance of product during manufacturing/packaging, testing, shipment, storage, or use. Such failures do not constitute a potential risk to the patient. The AQL for major defects normally ranges from 0.0 to 2.5 %.

What is Minor Defects :

It is one that will not affect the quality of the finished product (unsafe) and cause no potential risk to the patient. The AQL for minor defects normally ranges from 0.0 to 6.5 %.

Conclusion :

AQL is the additional control to know the defects of any Batch or Lot or container or Box but every employee or manufacturer or the organization should focused on quality of the drug products or materials during performing the activity online in order to have a better control on defects or Rejects which are generated from machine.

It means that we have to identify and correct the problems which may affect the quality of the compressed tablets, capsules and coated tablets during compression, Coating and capsule filling activity and management should be involved and take this seriously to avoid any market compliant or failure of the batch or Lot.