Month: December 2020

SOP for Analyst Qualification in Quality Control


1.0
Objective :
 To lay down a procedure for Training and Qualification of Quality Control Analyst.
2.0Scope :
 The scope of this document is to provide the procedure for Training and Qualification of Quality Control Analyst.
3.0Responsibility :
3.1Quality Control Personnel :
3.1.1To undergo Training and Qualification.
3.2Quality Control Head / Designee :
3.2.1To review and monitor the procedure for Training and Qualification of Quality Control Personnel.
5.0Procedure :
5.1Training shall be conducted by Manager / Designee for relevant core/ as per SOP, “Procedure for Training of Plant Personnel.
5.2Incase of SOP training the trainee shall be considered as ‘trained’ if analyst gets the qualifying score (> 80%) and should be evaluated through assessment questionnaire as per SOP, “Procedure for Training of Plant Personnel otherwise retraining shall be considered.
5.3Upon completion of training program, the new joinee shall undergo qualification process for all tests / techniques relevant to that area in which analyst is supposed to work.
5.4Based on the category to which the analyst belongs as per the discussion with the Head of Department, the tests in which the analyst shall be trained and qualified depending on the job responsibilities shall be identified.
5.5Non Complex Analytical Techniques are those for which a practical demonstration shall be provided by the trainer as per Annex – 1. As part of demonstration of these techniques, the Manager / Designee shall explain the test procedure to the analyst who is under training.
5.6Trainee shall enter the key learning points in the Analyst Qualification report.
5.7The details of the analytical techniques in which the analyst is trained and qualified shall be recorded in the current version of the “Analyst Qualification Record”,
5.8For complex analytical techniques the analyst shall be trained by Manager / Designee and key points of the analytical techniques shall be recorded by the trainer in “Analyst Qualification Record” during training.
5.9The analyst shall perform the test as per STP / Specification / GTP and qualification under the supervision of trainer and the qualification shall be verified as per the acceptance criteria.
5.10The trainer shall use the checklist provided in Annex – 3 to verify that the analyst undergoing qualification performs correct unit operations.        

5.11
Manager / Designee shall generate the Analyst Qualification Number (A.Q. No.) for each analyst as per procedure given below and this number shall be referred in analyst qualification raw data.
5.11.1AQXXYYY, Where AQ stands for Analyst qualification, XX denotes the last two digits of calendar year (20 for 2020) & YYY denotes the serial number.
5.11.2e.g. The Analyst qualification number for the first Analyst qualified in the year 2020 will be AQ20001
5.12For each analytical technique, the details such as “Name of Analytical Technique”, “Product” / “Material Name”, “Batch” / “Lot Number”, “A. R. Number” of the previous analysis shall be recorded in the “Analyst Qualification Register”.
5.13The details of analysis shall be recorded in the “Calculation Sheets” / “Test Data Sheets”. In case the qualification is performed on routine samples, the A.R. Number of the sample being analyzed shall also be recorded in the “Analyst Qualification Register” as a reference.
5.14The trainer shall review analytical results and consider the analyst as qualified, if the result of the test performed is complying with the acceptance criteria.
5.15Head of Department or his designee shall review the data of technique for which the analyst is under qualification and provide comments as “Qualified” or “Not Qualified” in the “Analyst Qualification Register”.
5.16At the beginning of every calendar year Manager / Designee shall prepare a schedule for re-training of relevant analytical techniques for each of the qualified personnel in the section in “Analytical technique Schedule”.
5.17The trainee shall be considered as trained only after the trainee qualifies as per the questionnaire.             
    5.18If the Analyst is having more than 2 years and above experience and have performed the similar analysis in previous organisation then depending upon the evaluation of previous experience and his expertise in the respective analytical technique, complex analytical technique need not be performed. In this case Analyst can directly put on the job by giving respective analysis of ongoing samples in presence of trained analyst and if the result meets the acceptance criteria then the analyst can be considered as Qualified Analyst.
 5.19Requalification of the Analyst shall be carried out if the analyst is absent for more than 60 working days.

6.0 Distribution :

This SOP (Controlled Copy) shall be distributed to Quality Control Department.

7.0 Annexures :

Annex-1 Non Complex Analytical Techniques for Qualification of Analyst

Annex-2 Complex Analytical Techniques for Qualification of Analyst

Annex-3 Checklist for Analyst Qualification.

8.0 Abbreviation :

Nil

9.0 Reference(s) :

Nil

10.0 SOP Revision History Record :

Revision No.Details for Revision(s) with Change Control No.Effective Date (Sign. / Date)

                                                               Annex-1

                           Non Complex Analytical Techniques for Qualification of Analyst

Sr. No.Analytical Technique
 1Description / Characteristics
 2Solubility of Solution
 3Appearance of Solution / Colour and Clarity of Solution
 4pH of Solution
 5Loss on Drying
 6Sulphated Ash
 7Residue on Ignition / Loss on Ignition
 8Heavy Metals
 9Limit tests such as Chloride, Sulphate, Nitrate, Lead, and Arsenic.
 10Bulk Density (Tapped / Untapped)
 11Distillation range
 12Melting Point
 13Sieve Analysis
 14Disintegration test
 15Friability
 16Thin Layer Chromatography
 17Preparation and Standardization of Volumetric solutions.
 18Determination of conductivity
 19Identification (FTIR, UV)

                                           Annexure-3    Checklist for Analyst Qualification                   
Name of the Analyst :
Product / Material/ Batch / Lot Number/ A. R.No.:
Test being performed:
Name of the Supervisor & Date:
Sr. No.ChecklistObservation     (Yes / No / NA)
 1Is the analyst using the correct analytical method for performing the analysis?  
 2Is the analyst using calibrated equipment / instrument for performing the analysis? 
 3Is the analyst using the correct working standard / reference standard? 
 4Is there evidence that the solutions/ reagents used during the analysis were within their validity period? 
 5Is it evident that the analyst is taking all the safety precautions? 
 6Is the analyst using the analytical balance correctly? 
 7Is the analyst using clean weighing accessories, like spatula, Butter paper, etc.? 
 8Is the solution prepared by the analyst labeled appropriately? 
 9Is the analyst using the correct glassware / reagents / chemicals / as mentioned in the analytical method? 
 10Is the analyst making concurrent documentation of the activity being performed? 
 11Are samples/ solutions stored appropriately during the analysis? 
Specific Observations for the Analytical Technique
    

Supervisor (Sign) & date:

Principle and working of Fluidized Bed Dryer (FBD)

What is Fluid Bed Dryer :

FBD is used for drying of different pharmaceutical materials or products and it can easily achieve specific moisture content in granules and powders.

FBD is able to remove excess moisture from different materials and its working principle is so precise and focused on drying the materials without changing their physical attributes.

FBD is used in different industries like Pharmaceutical, Chemical, Food Processing, Fertilizer and dairy industry.

What is the Purpose of Drying of Material in Pharmaceutical using FBD :

Here are the main functions as to why you should perform solid drying.

  • It increases the shelf life of the products
  • It helps in the improvement of different product properties such as compressibility and flow ability.
  • It will also make the materials more suitable for handling and it helps in proper preservation of the materials.

What is Fluidization Principle :

In fluidization process, hot air is introduced at high pressure through a perforated bed of moist solid particulate. The wet solids are lifted from the bottom and suspended in a stream of air (fluidized state). As the hot air passes between the particles it takes the excess moisture from the particles thus drying the particles.

Heat transfer is accomplished by direct contact between the wet solid and hot gases.

Steps of Fluidization :

Step 1: Fluidized bed dryer loading :

Loading of materials involves adding a fresh batch of wet granules into the product chamber through negative pressure feeding, materials can be sucked from the high shear  mixer chamber through a feeding tube.

Step 2: Air inlet (intake) :

Switching the blower unit on is done from the control panel. Once the blower is operational, the air is drawn continuously from the Air Handling unit and into the tower through the lower plenum.

Step 3: Fluidization :

Inlet air is blown up through the static power bed as the velocity of the air increases so does the space between powder particles until the particles become suspended in a bed the fluidization process is through to occur in five stages including smooth  fluidization, bubbling  fluidization, turbulent fluidization and first  fluidization.  

Step 4: Drying:

The drying process takes place in three stages until the end point is reached (At the end point the solid particles moisture level is equal or less than 1%)

Step 5: Pre heating:

Wet particles are suspended in hot and dry air stream. Moisture on the particles surface evaporates as heat flows through the body  (conventional heating) the rate of drying slowly increases as the particles absorb more heat.

The moisture lost during preheating is still small but the temperature of the bed rises steadily.

Step 6: Filter bag shaking:

The blower continuously draws and excels air from Fluidized bed dryer. The airstream may contain very small particles called fines. The filter bags capture the fines in their pores but this cause the formation of a dust layer that clogs the filter bags causing a pressure drop.

Mechanical shaking is the best way to remove the dust layer and it is done by the pneumatic cylinder at the set intervals and seems we have two filtering chamber the shaking is alternated between the two.

Refer Fluid Bed Dryer Filter Bag

https://pharmaceuticalupdates.com/2020/10/05/procedure-for-indent-receipt-usage-and-specifications-of-fluid-bed-drier-filter-bag/

 Step 7: Discharging of dried material:

Discharging refers to the removal of dried materials from fluidized bed dryer. It can be done manually by unlocking and wheeling the product container on its trolley to the next process equipment.

Alternatively, vacuum conveying can be carried out by connecting the product container with a tube and creating negative pressure for suction using a vacuum transfer system. After drying, the next process is milling.

What are the main disadvantages of using the fluid bed dryer :

Not Ideal for Organic Solvents :

You cannot use the fluid bed dryer for reducing excess moisture in organic solvents or substances containing organic solvents.

This is because the organic solvents usually dissolve in the products thus making it very difficult to dry.

Risk of Fire Explosion:

Fluid bed dryers use high levels of hot gas and air thus making it difficult to dry toxic or flammable materials.

This may place the lives of the people operating the machine or around the machine in great danger.

Electrostatic Build-up :

When we use the fluid bed dryer there are high chances of electrostatic build up during the drying process.

It is a phenomenon that will happen especially when we are drying organic particles.

We should, therefore, go for the fluid bed dryers with electrical earthing elements to avoid this problem.

Difficulty in Drying Sticky Particles :

The main principle of drying using the fluid bed dryer is the movement of particles as it takes away excess moisture.

We will, therefore, experience a lot of problems when it comes to drying sticky materials as they don’t move freely.

Material of Construction of FBD:

For the contact parts of FBD we should use  AISI 316 and non-contact parts AISI 304.

Fluid Bed Dryer Quality Standards and Certifications:

The main quality standard and certification are

  • Current Good Manufacturing Practices (cGMP)
  • International Standards Organization (ISO) Quality Certification
  • Food and Drug Administration Quality Certifications
  • CE quality certification for the electrical appliances

Procedure for Operation of Friabilator Make: Electro lab

  1. OBJECTIVE

1.1 To lay down a procedure for operation of Friabilator, Make: Electro lab

2.0       RESPONSIBILITY

2.1 Technical Assistant / Production Executive / IPQA Executive – To Perform as per SOP.

2.2 Production / IPQA In-charge – To ensure the compliance.

3.0 PROCEDURE

3.1   OPERATION :

3.1.1     Switch ON the mains.

3.1.2    Press the START/STOP switch on the rear right hand side of the instrument base, then the drum will initialize itself to the loading position and simultaneously display shows START.

3.1.3 Mode setting – TIME, COUNT key are toggle keys to set in Timer mode or Count mode of operation.   3.1.4   Set the Time in the following procedure:

 3.1.4.1  Press “RESET” key.

 3.1.4.2  Press “TIME” key.

 3.1.4.3  Enter the required duration of time by pressing the numeric digits.

 3.1.4.4  Press “ENTER” key to set the time.

3.1.5     Set the Count in the following procedure:

  3.1.5.1  Press “RESET” key.

  3.1.5.2  Press “COUNT” key.

  3.1.5.3  Enter the desired number of rotations by pressing the numeric digits.

 3.1.5.4  Press “ENTER” key to set the count.

 3.1.5.5  After completing the parameter settings, slide the tablets gently into the drum from the side slit provided on the drum. 

3.1.5.6  Select the Time mode or Revolution count mode as desired by pressing the “TIME / COUNT” key respectively.

PRECAUTIONS:

  1. Make sure the knob is properly fitted on the shaft to assure the drum is held in position.
  2. Do not hold the drums while they are rotating.

3.1.6 Weigh the quantity of tablets to be tested as per the BPRR specification from LHS and RHS of compression machine.

3.1.7 Record the weights of tablets in BPRR if provided and load the tablets to  friabilator drum.

3.1.8 Press “RUN / HALT” key to start the test.  “RUN / HALT” is a toggle key to start and stop the test.

3.1.9 Drums rotate in forward direction as per the set (TIME/COUNT) mode.

3.1.10 Completion of test is indicated by an audible beep and the display shows “END”.

3.1.11 When the test is over, the drums rotate in the reverse direction for discharging the tablets into the trays.  After discharge of tablets drums initialize to loading position and the display shows “START” indicating the instrument is ready for next test.

3.1.12 Slide out the tray and take out the samples for weighing.

3.1.13 Dedust the tablets using nylon brush, weigh and record  in BPRR.

3.1.14 Calculate and record the friability as per BPRR.

Note:

  1. If tablet size or shape causes irregular tumbling, adjust the drum base so that the base forms an angle of about 100 with the table surface and the tablets no longer bind together when lying next to each other, which prevents them from falling freely.
  2. Adjustment of the drum base can be done by opening the two flaps, which are situated at the front bottom side of the instrument.

3.2    CLEANING :

3.2.1     Clean the Friabilator frequently by following procedure.

3.2.2     Switch off the power supply to the instrument before cleaning the equipment.

3.2.3     Remove the trays in the tray holders.

3.2.4     Remove the drums from the shaft by pressing the button on the knob and pull   out  the knob.

3.2.5 Clean the drums, trays and knob with lint free cloth dipped purified water and wipe with dry lint free cloth.

3.2.6 Wipe off the exterior of the equipment with lint free wet cloth.

3.2.7 Reassemble the drums and tray in the reverse order of dismantling.

3.2.8 Update the status label as CLEANED.

3.2.9 Switch off the mains of the tablet friability apparatus after the days operation.

Frequency   :   After every batch irrespective of product, or Weekly (if machine is in

operation), or Monthly (if machine is idle) which ever is the earlier and as and when   required.

4.0       ABBREVIATIONS

Nil

5.0       REFERENCES

Nil

6.0       ANNEXURES

Nil

Review of Audit Trails in Laboratory Systems

What is Audit Trail :

An audit trail or  audit log is a security-relevant chronological record, set of records, or destination and source of records that provide documentary evidence of the sequence of activities that have affected at any time a specific operation, procedure, or event. 
Audit trail means a secure, computer-generated, time-stamped electronic record that allows for reconstruction of the history of events relating to the creation, modification, or deletion of an electronic record.
For example, the audit trail for a high performance liquid chromatography (HPLC) run should include the user name, date/time of the run, the integration parameters used, and details of a reprocessing, if any.
Audit trail should be available in analytical instruments like High performance liquid chromatography (HPLC) , Gas chromatography (GC), Infrared Spectrophotometer, Ultra Violet Spectrophotometer, Water By KF etc.

The review of Audit Trails in Laboratory Systems may include the following verification but not limited to :

For more details pl refer Requirement of Audit trail in Pharmaceuticals

https://pharmaceuticalupdates.com/2020/05/06/requirement-of-audit-trail-in-pharmaceuticals-and-in-other-industries/

Operation of Disintegration test Apparatus Make : Electro lab

1.0       OBJECTIVE

             1.1         To lay down a procedure for operation of Disintegration test apparatus, Make: Electrolab

2.0       RESPONSIBILITY

2.1        Technical Assistant / Production Executive / IPQA Executive – To perform as per SOP

2.2        Production / QA in-charge  – To ensure the compliance

3.0       PROCEDURE

3.1 Operation     

3.1.1 Switch on the mains.

3.1.2 Press the START/STOP switch on the rear right hand side of the instrument base.

3.1.3 TIMER key is a toggle key to set Timer mode or Manual mode of operation.   Incase of Manual mode the display shows ‘——’ and the apparatus run irrespective of the set time value. Incase of the Timer mode the apparatus is switched off automatically after the set time value of the test..

3.1.4 Check that the water bath  is filled with purified water  up to the level marked.

3.1.5 Beakers are filled with freshly collected purified water, adjust the volume of purified water , such that when the assembly is in highest position the wire mesh is at least 15mm below the surface of purified water and when the assembly is in lowest position the wire mesh is at least 25mm. above the bottom of the beaker and upper ends of the tubes remains above the surface of purified water.

3.1.6 Set the temperature in the following procedure.

  • Set the temperature 37 ± 20C , unless specified in the BPRR.
  • Press “SET” Key.
  • Press “TEMP” Key.
  • Press “DISP. SEL” Key to select the digit to be changed.
  • Press either “D” or “Ñ“ Key to attain the desired temperature.
  • Press “ENTER” Key to set the temperature.
  • The “TEMP” key is a toggle key used to start and stop the temperature controller.

3.1.7 Set the time in the following procedure.

  • Select the timer in MIN: SEC range by pressing the key SET, ENTER simultaneously.   Incase of HRS: MIN the display shows a “-” before time.   
  • Press “SET” Key.
  • Press “TIMER” Key.
  • Press “DISP. SEL” Key to select the digit to be changed.
  • Press either “D”  or “Ñ”key to attain the desired temperature.
  • Press “ENTER” Key to set the timer.
  • “START / STOP” key is toggle key for the timer.

3.1.8 After completing the parameter settings start the temperature controller by pressing “TEMP” key.

3.1.9 Select the bath temperature indicator using PROBE / SEL key.  Once the bath temperature achieves the set value the instrument is ready to use.

 Precaution

The external probe should be handled carefully. When the external probe is not in use, keep it in  the place provided for it on the bath

3.1.10 Press the START / STOP key to start the test.

3.1.11 Take sufficient quantity of tablets / capsules to be tested as per the BPRR.

3.1.12 Place one tablet / capsule in each cylinder of the basket followed by disc  ( If required )

3.1.13 Observe the tablet / capsule to disintegrate completely through the mesh.

3.1.14 Press START / STOP Key to stop after complete disintegration of tablet / capsule.

3.1.15 Record the time shown in the timer in BPRR.

3.1.16 Remove the basket assembly from the hook arm and replace the water in the beaker  before proceeding for next test.

3.2 CLEANING

3.2.1     After Every Test :

3.2.1.1 Switch off the power supply before starting the cleaning activity.

3.2.1.2 Remove the basket assembly by disengaging from the hook arms and remove the beakers   from the acrylic water bath.

3.2.1.3 Wash the beakers, baskets, discs and top plate with purified water.

3.2.1.4 Wipe the body of the disintegration test apparatus using lint free cloth dipped in purified water.

3.2.1.5 Collect purified water in beakers and reassemble the beakers and baskets.

3.2.2    Weekly Cleaning :

3.2.2.1  Switch off the power supply before starting the cleaning activity.

3.2.2.2  Remove the basket assembly by disengaging from the hook arms and remove the beakers   from the acrylic water bath.

 3.2.2.3   Disconnect the heating coil plug to the water bath from rear side of the apparatus.

 3.2.2.4   Detach the water bath from the apparatus base

3.2.2.5  Wash the water bath, beakers, baskets, discs and top plate with purified water.

3.2.2.6  Wipe the body of the disintegration test apparatus using lint free cloth dipped in purified water. 

3.2.2.7  Collect purified water up to the marked level and reassemble the water bath and top plate in the reverse procedure of dismantling.

3.2.2.8   Collect purified water in beakers and reassemble the beakers and baskets.

3.2.2.9   Update the status label as “CLEANED”.

3.2.2.10 Switch off the power supply of the instrument after the days operation.

PRECAUTION

  1.   Make sure that the heater is connected properly.

2.  Do not try to remove the basket until it is disengaged from the hook arm.

4.0       ABBREVIATIONS

             Nil

5.0       REFERENCES

Nil

6.0 ANNEXURES

Nil