ORAL DOSAGE FORM SOPs

1.0 PURPOSE

To lay down a procedure for Preparation of stock solution to be used for limit test. 

2.0 SCOPE: 

This procedure is applicable to Preparation of stock solution for limit test like heavy metals, chloride, sulphate, nitrate in the quality control Laboratory.

5.0 PROCEDURE:

5.1 Stock solution shall be prepared from the 1000 ppm solution or 100 ppm solution of the particular standard solution or as specified in pharmacopoeia

5.2 Once the stock solution is prepared it can be used upto 3 months from the date of preparation.

5.3 The standard stock solution should not be contaminated at the time of pipetting the solution.

5.4 Material safety data shall be referred whenever required.

5.5 When any precipitation is observed before the expiry date the same solution shall be discarded.

5.6 Assign the ID no. of Standard solution in following manner SS-XX/x/yy

          where:

        SS             :     Standard  Solution

        XX           :     Code  number 

        x               :      Serial No

          YY           :     Year

5.7 Transfer the Standard solution from the volumetric flask to clean and dry stopper bottle.

5.8 Put a label with all the details as per Annexure – 1

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1.0 PURPOSE

To lay down a procedure for preparation of reagents solution and Indicators.

2.0 SCOPE: 

This procedure is applicable for the preparation of reagents, solutions and Indicators in Quality Control Department.

5.0 PROCEDURE:

5.1 Prepare reagent solutions and indicators as per respective pharmacopoeia

5.2 Use distilled water for preparation of reagent solution and indicators.

5.3 Use AR/GR/LR grade reagent for preparation of reagent solution or indicators.

5.4 Assign the ID no. of reagent solution/ indicator in the the following manner TS/I-XX/x/yy

Where TS: Test solution, I: Indicator

XX:  Code number

x:    Serial number

yy: Year

5.5 Transfer the Reagent/Indicator from the volumetric flask to clean and dry stopper bottle. Put a label with all the details as per Annexure - I

5.6 The expiry date of reagent solution and indicator is 3 months from the date of preparation.

5.7 Reagent solutions must be stored in colourless / amber colour glass bottles with lid as per requirement.

5.8 Discard the solution immediately if any contamination, decolouration, sedimentation observed in the solution

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1.0 PURPOSE3

To lay down a procedure for Retesting of Raw materials.

2.0 SCOPE:

This procedure is applicable to Retesting of Raw materials in quality control department.

5.0 PROCEDURE:

5.1 Sampling of Raw materials and due for Retesting

5.1.1 Retesting of raw material shall be initiated after receiving the intimation from stores department.

5.1.2 Stores department shall transfer the retest material in UNDER TEST area and deface the approved labels on the container by putting the cross mark on the label.

5.1.3 Retest period/date should not exceed the actual expiry date declared by manufacturer or use before in case of flavour. It is preferred to carry out the test before 7 days; in this case transfer of material to under test shall be avoided.

5.1.4 Analyst/Designee QC shall enter the material details in raw material retest inward record and shall assign new A.R. No. by putting a suffix R1,R2, R3 for each batch /lot to the original A.R. No. of Raw materials for retesting 1^st time, retesting 2^nd time and retesting 3^rd time respectively as per Annexure-1.

5.1.5 Analyst/Designee QC shall prepare Under test labels as per received intimation slips for each container.

5.1.6 Analyst/Designee QC shall enter in the stores department under-test area along with sampling kit.

5.1.7 Analyst/Designee QC shall perform the sampling as per raw materials sampling in respective area.

5.2 Sampling Plan

5.2.1 Sampling has to be performed from the container, which had been taken for dispensing, if no such Container is found, sampling has to be performed from any one of the container of the Batch.

5.2.2 Analyst/Designee QC shall mark “sampled” on each sampled container for analysis.

5.2.3 Analyst/Designee QC shall perform the test of Raw materials as per respective standard test procedures and specifications.

5.2.4 After completion of analysis, all data shall be reviewed and certificates of analysis for each batch shall be prepared.

5.2.5 If material is approved prepare Approved labels for all containers as per Sampling of Raw materials.

5.2.6 If materials is rejected as per the Specification, Re-sampling has to be done and Tested as per Specification.

5.2.7 If materials is rejected prepare Rejected labels, and affix on each packs on the particular batch below the “Under test label”. Initiate the “Rejection Note” for respective materials.

5.2.8 Send the rejection note to warehouse and ensure that the material is transferred to Rejected area.

5.3 Frequency for Retesting of Raw Materials

5.3.1 All Active Raw materials shall be retested after one year from the date of Release.

5.3.2 All Inactive raw materials (excipients) shall be retested after two year from the date of Release.

5.3.3 All vitamins shall be retested after six months from the date of Release.

5.3.4 All liquid flavours (excipients) shall be retested after six months from the date of Release.

5.3.5 All solid flavours (excipients) shall be retested after one year from the date of Release.

5.3.6 After getting intimation from stores department for retesting, arrange for sampling.

5.3.7 Sample the material and perform tests as per specification.

5.3.8 Paste approved label after completion of analysis, if found within limit and rejected label if found out of the limits. Inform to the Head Quality Control.

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1.0 PURPOSE

To provide a procedure for Handling of Out of Specification Results.

2.0 SCOPE: 

This procedure is applicable to Quality Control laboratories. This procedure applies to all analytical results that fall outside the specification or acceptance criteria of raw materials (API, Excipients and Pre-shipment sample etc.); Intermediates, recovered solvent, In-process samples, Semi-Finished Products and Finished Products.

The principles of the procedure are also applicable to the following:

1. Analytical tests involved in validation studies.
2. Stability testing.
3. Environmental monitoring / water monitoring results exceeding action limits.
4. Microbial Limit test.
5. Physical parameters of product which includes In-process samples, semi-finished products / Intermediates, finished products, stability samples and validation samples, Cleaning Validation etc.
6. Packaging materials.
7. Water samples
8. Hold time

5.0 PROCEDURE:

5.1 IDENTIFICATION OF OOS:

5.1.1 Analyst shall complete the analysis of sample for the relevant tests or all tests as per STP/Protocol. The calculated test results shall be verified for the compliance against respective specification. If any of the result is not meeting the specification or acceptance criteria, the test result is considered as OOS result and the analyst shall inform the OOS result to Supervisor QC. Document immediately in the analytical records and take photograph wherever applicable. Do not continue any analysis that will be invalidated at a later stage, for an assignable cause.

5.1.2 Analyst/Supervisor shall log the OOS within one working day, from the date of observation. Analyst shall freeze the bench top solutions, laboratory equipment and retain/store the Standard and test preparations as per the recommended storage condition to prevent the degradation till the completion of Preliminary Investigation.

5.1.3 Investigation of OOS results shall be done in two phases:

         Phase I:Preliminary/Laboratory Investigation

         Phase II : Additional laboratory Investigation and Manufacturing process review

5.1.4 Phase I Investigation allows to determine if there is an obvious error and generally includes initial assessment of accuracy of laboratory data.

Note: In case of obvious errors listed below but not limited to:

• Calculation error
• Power outage, equipment failure
• Testing errors like spillage of solution, incomplete transfer of a sample composite
• Incorrect Instrument parameters

5.1.5 Phase II Investigation includes additional laboratory investigation and manufacturing process review to identify the root cause and take appropriate CAPA.

5.1.6 Lab Phase I – Section A:

• Supervisor / Analyst (Originator) shall fill the below mentioned information in the OOS.

Forms as per phase 1 –Section A

Microbiological based OOS results:

• The test results which are not meeting the acceptance criteria for the tests such as Total microbial count, Microbial assay/dissolution/water/Pathogens, EMP etc. shall be considered as Microbiological based OOS results.

Chemistry based OOS results:

• The test results which are not meeting the acceptance criteria for the tests such as identification, solubility, related substances, limit tests, assay, residual solvents, preservative content, etc. shall be considered as Chemistry based OOS results;
• For the test parameters Dissolution and Uniformity of Dosage units (Content Uniformity by Assay & weight variation), if the dissolution test results are not meeting the S1 acceptance criteria and the Uniformity of Dosage units (Content Uniformity by Assay & weight) test results are not meeting the L1 acceptance criteria.

Physical parameter based OOS results:

• The test results which are not meeting the acceptance criteria for physical parameters of a product or physical parameters of packaging material, periodic review of reserve / control sample shall be considered as Physical parameter based OOS results.
• Invalidation of initial OOS test results should be justified with the help of suitable supporting data and / or statistical evaluation.

5.1.7    If OOS is wrongly logged or is not required or in case of duplication of OOS raised for the same      failure inadvertently, Quality Control Supervisor or designee shall provide the adequate      justification for cancellation. On review Head –QA or designee shall cancel the record with      adequate justification.

5.1.8    QA shall write activity as “Cancel”, update justification for cancellation in summary and the           record will be “Closed Cancelled”.

5.1.9     Originator shall submit, the dully filled OOS forms to QA.

5.1.10  If any information is inadequate or any modifications required, the form shall be sent back to   originator.

5.1.11   Lab Phase I – Section B:

5.1.11.1 If the OOS record is to be proceeded further, Supervisor shall write the activity as “Phase I initiated”  and the record of “Phase I Under Progress” and fill the following fields under Lab Phase I – Section

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1.0 PURPOSE

To lay down a procedure for operation of Hot plate.

2.0 SCOPE: 

This procedure is applicable for operation of Hot plate in the Quality control department.

5.0 PROCEDURE:

5.1 Operation:

5.1.1 Ensure that instrument is clean and free from dust.

5.1.2 Switch on the mains.

5.1.3 Adjust the thermostat to the required temperature by moving it in a clockwise direction.

5.1.4 Keep the vessel containing solution on the instrument to heat.

5.1.5 After heating, turn the thermostat knob to zero and off the mains when the temperature comes down to 40°C – 45°C.

6.0 ENVIRONMENT HEALTH AND SAFETY PROTECTION

6.1       Do not spill any organic solvent on the instrument.

6.2       Clean the instrument properly after use.

6.3       Put the main switch off only when the temperature comes down to 40°C- 45°C.

6.4       Do not ON the instrument if any inflammable reagent falls on it.

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1.0 PURPOSE

To lay down a procedure for Operation of Magnetic stirrer.

2.0 SCOPE: 

This procedure is applicable to stir tin the Quality Control Department.

5.0 PROCEDURE:

5.1 Operation:

5.1.1 Ensure that instrument is clean and free from dust.

5.1.2 Switch on the mains.

5.1.3 Set the high speed or low speed level by switch.

5.1.4 Adjust the required temp by moving knob in a clockwise direction

5.1.5 Adjust the speed to the required by moving it in a clockwise direction.

5.1.6 Keep the vessel containing solution on the Instrument with stirrer.

5.1.7 After complete of work turn the knob to zero and after 15-20 minutes put off the main switch.

5.1.8 Record the details in the instrument log book for results and breakdown.

6.0 ENVIRONMENT HEALTH AND SAFETY PROTECTION

6.1 Do not spill any organic solvent on the instrument.

6.2 Clean the instrument properly after use.

6.3 Put the main switch off only when the temperature comes down to 40°C-45°C.

6.4 Do not ON the instrument if any inflammable reagent falls on it .

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1.0 PURPOSE

To lay down a procedure for operation of ultrasonic bath.

2.0 SCOPE: 

This procedure is applicable to operation of ultrasonic bath in Quality Control Department.

5.0 PROCEDURE:

5.1 Operation:

5.1.1 Ensure that instrument is clean and free from dust.

5.1.2 Switch on the mains.

5.1.3 Add nearly 2-inch height water to the tank.

5.1.4 Switch on the instrument.

5.1.5 The knob at front panel is for temperature control. The glowing of pilot lamp indicates the heater’s “ON” position, pilot lamp will go "OFF" as soon as desired temperature is attained.          

5.1.6 The instrument will dissolve the solid in solvent or mix the solution properly by Ultrasonic Wave effect. Put OFF the instrument after use.

5.1.7    Record the details in the instrument log sheet. If any deviations are observed in the instrument, inform the Head Quality control department and call the Service Engineer.

6.0 ENVIRONMENT HEALTH AND SAFETY PROTECTION

6.1 Do not overload the tank with too many samples.

6.2 Do not switch on any controls when the tank is empty.

6.3 Cleaning should be done with water Frequently.

6.4 Do not put the inflammable solution, strong acid in Ultrasonic bath when heater in use.

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1.0 PURPOSE

To lay down a procedure for operation of Muffle furnace.

2.0 SCOPE: 

This procedure is applicable to operation of Muffle furnace in the Quality Control Department.

5.0 PROCEDURE:

5.1 Operation:

5.1.1 Ensure that instrument is clean and free from dust.

5.1.2 Keep muffle furnace in normal vertical position

5.1.3 Switch ‘ON’ the mains.

5.1.4 Load the material into the furnace and close the door firmly.

5.1.5 Switch on instrument, which will be indicated by glow of the green lamp.

5.1.6 Set the desired temperature by moving the knob to the left side.

5.1.6 Set the temperature by rotating the temperature control knob in clockwise direction.

5.1.7 When temperature is set to the desired value again move the set knob to its original position.

5.1.8 Wait for some time and allow few operations for energy regulator for ON and OFF cycle of furnace.

5.1.9 If the temperature is less or falling then increase the temperature by turning  the temperature knob button.

5.1.10 Wait for sometime and observe the temperature from time to time  in order to maintain   required  temperature .

5.1.11 Record the details in the instrument log book for results & breakdown.

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1.0 PURPOSE

To lay down procedure of operation of Mechanical Sieve shaker.

2.0 SCOPE: 

This procedure is applicable for the Sieve shaker used in Quality Control laboratory.

5.0 PROCEDURE:

5.1 Operation:

5.1.1 Ensure that instrument is clean.

5.1.2 Fix the rods on the top plate of instrument and ensure that they are tightly fitted.

5.1.3 Loosen the sieve clamp knob till the rubber pan holder touches the horizontal bar.

5.1.4 Loosen both the rod clamping knob.

5.1.5 Place the material to be sieved in to the sieve.

5.1.6 Place the horizontal bar above the sieves so that the rubber pad touches the sieve.

5.1.7 Lock the bar to the vertical rod by turning the rod clamping knob in clock wise direction

5.1.8 Now lock both the sieve clamp knob by turning it in clock wise direction

5.1.9 Switch “ON” the main supply; switch “ON” the instrument.

5.1.10 Set the desired time by TIMER key.

5.1.11 Control the speed by rotating the speed knob in clock /anti clockwise direction.

5.1.12 Switch Off the instrument, after sieving is finished.

5.1.13 Record the activity in mechanical Sieve shaker operation log book as per annexure -1

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1.0 PURPOSE

To lay down a procedure for cleaning, operation and monitoring of Refrigerator.

2.0 SCOPE: 

This procedure is applicable for cleaning, operation and monitoring of refrigerator in the quality control department

5.0 PROCEDURE:

5.1 Cleaning

5.1.1 Switch off the refrigerator.

5.1.2 Remove all the material from the refrigerator.

5.1.3 Mop it with 70% v/v IPA soaked cotton

5.1.4 After evaporating of IPA mop it with 20% v/v solution of virosil.

5.1.5 Wipe it with soft dry cloth and record the detail as per Annexure-1

5.1.6 Frequency of Cleaning: Once in a month

5.2 Operation.

5.2.1 Switch “ON” the refrigerator.

5.2.2 Set the knob ‘max’ to get the required temperature.

5.2.3 Shut the door of refrigerator properly.

5.2.3 Monitoring

5.3.1 Observe and record the temperature daily with the help of calibrated thermometer placed inside the chamber as per Annexure-2

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