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In process Quality Control (IPQC) Check Procedure – Guidelines – SOPs

Standard Operating Procedure (SOP) for In process Quality Control (IPQC) checks performed at different stages during manufacturing of pharmaceuticals drug product.

What is IPQC : IPQC (In Process Quality Control) is the controlling procedures involved in manufacturing of dosage forms starting from raw material purchase to dispatch in final packaging.

In process Quality Control (IPQC) checks

1.0   Objective :

    • To lay down procedure for checking of in-process parameters of Oral Liquids, Tablets & Capsules.

2.0   Scope :

    • The SOP is applicable in Production during capsule filling, liquid filling, compression, coating & packaging at pharmaceuticals plant.   

3.0   Procedure – In process Quality Control (IPQC) :

  • Disintegration Test (DT) :

    • What is Disintegration Test:

    • Disintegration is defined as that state in which no residue of the tablet or capsule remains on the screen of the apparatus or,

    • If a residue remains, it consists of fragments of insoluble coating of the tablets or of capsule shells or is a soft mass with no palpable core.

    • What is Tablets:

    • Tablets are solid dosage forms each containing a unit dose of one or more medicaments.

    • They are intended for oral administration.

    • What is Capsules:

    • Hard Gelatin Capsule Shells are soluble containers for incorporation of drugs, usually in the form of powders, pellets, or granules, and are commonly intended for oral administration.

    • Requirement For Disintegration Test During In Process Quality Control (IPQC):

    • SOP for Operation and Calibration of DT Apparatus

      Disintegration Test Apparatus

    • Thermometer

    • Water / as specified

    • Method (Procedure) for Disintegration Test:

    • Sample Quantity: 6 tablets / 6 capsules

    • Add approx. 800 ml water (or as specified) in a 1-litre beaker and place in the water bath.

    • Wait till the temperature of water / specified solvent reaches up to 37±2°C.

    • After maintaining the temperature, introduce one tablet / capsule in each tube.

    • Place the disc in each tube or as specified.

    • Suspend the assembly in the beaker containing water / specified solvent.

    • Operate the apparatus as per SOP.

    • Record the time at which all the tablets / capsules disintegrate.

    • Acceptance Criteria for DT Test:

    • No residue of the tablet or capsule remains on the screen of the apparatus or, if a residue remains, it consists of fragments of insoluble coating of the tablets or of capsule shells or is a soft mass with no palpable core.

    • All the six tablets / capsules must pass the test.

    • If 1 or 2 tablets or capsules fail to disintegrate, repeat the test on 12 additional tablets or capsules; not less than 16 of the total of 18 tablets or capsules tested disintegrate.

    • Note: If the tablets or capsules adhere to the disc and the preparation being examined fails to comply, repeat the test omitting the disc.

    • The preparation complies with the test if all the tablets or capsules in the repeat test disintegrate.

    • Disintegration Test of Uncoated Tablets:

    • Medium : Water or as specified

    • Use disc to each tube.

    • Temperature: 37 ± 2°C

    • Limit: NMT 15 Minutes or as specified

    • Disintegration Test of Film coated Tablets:

    • Medium : Water or as specified

    • Use disc to each tube.

    • Temperature: 37 ± 2°C

    • Limit: NMT 30 Minutes or as specified

    • Disintegration Test of Gastro resistant (Enteric Coated) Tablets:

    • Medium : Ist : 0.1 M Hydrochloric Acid IInd : Mixed Phosphate Buffer pH 6.8 or as specified

    • Temperature: 37 ± 2°C

    • In 0.1 M Hydrochloric Acid: NLT 2 hours.

    • Operate the apparatus without disc for 2 hours.

    • Remove the

      assembly from the liquid.

    • No tablet shows signs of cracks that would allow the escape of the contents of

      disintegration, apart from fragments of coating.

    • In Mixed Phosphate Buffer pH 6.8: NMT 60 minutes.

    • Replace the liquid in the beaker with mixed phosphate buffer pH 6.8,

    • Add a disc to each tube, and operate the apparatus for a further 60 minutes.

Read Also : Analytical Method Transfer

    • Remove the assembly from the liquid.

    • If the tablets fails to comply because of adherence to the disc, repeat the test on a further 6 tablets without discs.

    • The tablets pass the test if all six have disintegrated.

    • Disintegration Test of Dispersible Tablets:

    • Medium : Water or as specified

    • Use disc to each tube.

    • Temperature: 24 – 26°C

    • Limit: NMT 3 Minutes or as specified

    • Disintegration Test of Orally Disintegration Tablets:

    • Medium : Water or as specified

    • Use disc to each tube.

    • Temperature: 24 – 26°C

    • Limit: NMT 3 Minutes or as specified

    • Disintegration Test of Hard Gelatin Capsules:

    • Medium : Water or as specified

    • Temperature: 37±2°C

    • If the capsules float on the surface of the medium, a disc may be added.

    • If the capsules adhere to the

      discs, attach a removable piece of stainless steel woven gauze with mesh aperture of 2 mm to the upper plate of the basket rack assembly and carry out the test omitting the discs.

    • Limit: NMT 30 Minutes or as specified.

  • Friability Test – During In Process Quality Control (IPQC) :

    • Definition of Friability :

    • The phenomenon whereby tablet surfaces are damaged and/or show evidence

      of lamination or breakage when subjected to mechanical shock or attrition.

    • Expression of Result : % w/w

    • Requirement for Friability Test during In process Quality Control (IPQC):

    • Weighing Balance

    • Method (Procedure) Friability Test:

    • Sample Quantity:

    • For tablets with an average weight of 0.650 g or less take a sample of whole tablets to about 6.50 g and for tablets with an average weight of more than 0.650 g take a sample of 10 whole tablets.

    • Remove any loose powder using soft brush from the tablets to be tested.

    • Accurately weigh the tablets & record the weight in gram (A).

    • Load the tablets in to the drum and operate the apparatus following respective SOP for 100 rounds.

    • After completion of test, unload the tablets and brush away any loose powder from them.

    • Accurately weigh the tablets and record the weight in gram (B)

    • Calculation o

      f

      Friability Test:

                                             [A] – [B]          

                     Friability = ———————x 100

                         [A]

    • Acceptance Criteria of Friability Test:

    • Not more than 1 % w/w

    • If cracked, cleaved or broken tablets are present in the tablet sample after test, the sample

        

    • If the weight loss is greater than 1 % w/w, repeat the test twice and the mean of 3 tests

      determined. This should not be greater than 1 %.

  • Determination of Hardness of Uncoated Tablets or Resistance to crushing of tablets during In process Quality Control (IPQC):

    • Definition:

    • Under defined conditions, the resistance to crushing of tablets, measured

      by the force needed to disrupt them by crushing

    • Expression of Result : Newton (N) / kg / cm2

    • Requirement:

    • Hardness Tester

    • Method:

    • Sample Quantity: Take 10 tablets.

    • Measure the hardness of 10 tablets with the help of Hardness Tester.

    • Take the mean of 10 tablets.

    • Operate hardness tester as per SOP.

    • Note: Remove all the fragments of the tablets before each determination.

    • Acceptance Criteria: The mean of 10 tablets should not be less than as specified.

  • Measurements of Dimensions of Tablets:

    • Expression of Result :  mm (millimeter)

    • Requirement:

    • Vernier caliper

    • Method:

    • Sample Quantity: Take 10 tablets

    • Measure diameter & thickness for round tablets, length, width & thickness of elongated, oval, elliptical tablets.

    • Operate the vernier caliper as per SOP.

    • Acceptance Criteria: All the readings of 10 tablets should be within limit as specified.

  • Determination of Average Weight / Average Fill Weight / Uniformity of weight / Uniformity of fill weight:

    • Average Weight:

    • Equipment: Analytical Balance

    • Applicability : Applicable for all type of tablets

    • Operate the analytical balance as per SOP.

    • Take the disc / SS bowl and place on the pan and tare

    • Take 20 tablets from the composite sample, place on disc / SS bowl and record the weight.

    • Calculation:

           Weigh of 20 tablets (g)

=…………………………………

    20

    • Limit : As per MFR / BMR

  • Uniformity of Weight:

    • Equipment: Analytical Balance

    • Applicability: This test is applicable for uncoated and film coated tablets.

    • Operate the analytical balance as per SOP.

    • Take the disc / SS bowl and place on the pan and tare it.

    • Take 20 tablets from the composite sample.

    • Place one tablet on the disc / SS bowl and record the weight.

    • Tare it and place the second tablet and record the weight.

    • Repeat the procedure with a further 18 tablets.

    • Acceptance Criteria:

    • None tablet should deviates by percentage given below or as specified in BMR.

    • In critical case not more than two of the individual weights deviate from the average weight

      by more than the percentage given below and none deviates by more than twice that

      percentage or specified in the BMR.

Average Weight of Tablets

Percentage Deviation

80 mg or less

10

More than 80 mg but less than 250 mg

7.5

250 mg or more

5

  • Calculation of % Variation:

                                  Min. wt. of Tablet – Average weight)

% Minimum Variation = ————————————————— x 100

                    Average Weight

 

                                        (Max. wt. of Tablet – Average weight)

% Maximum Variation = ————————————————— x 100

                           Average Weight

  • Average Fill Weight – In process Quality Control (IPQC) :

    • Equipment: Analytical Balance

    • Applicability: Applicable for hard gelatin capsules

    • Operate the analytical balance as per SOP.

    • Take the disc / SS bowl and place on the pan and tare it.

    • Method :

    • Place 20 capsules and records the weight.

    • Open all the 20 capsules without losing any part of the shell and remove the contents as completely as possible.

    • Weigh all the 20 empty capsule shells and record the weight.

    • Calculation:

Weight 20 filled capsules – weight of 20 empty capsules

=——————————————————————————-

20

    • Method II :

    • Add the weight of content of 20 capsules (determined under uniformity of fill weight).

    • Calculation:

                              Weight of content of 20 capsules

            =————————————————–

       20

    • Limit : As per MFR / BMR

  • Uniformity of fill Weight – In process Quality Control (IPQC) :

    • Equipment: Analytical Balance

    • Applicability: This test is applicable for hard gelatin capsules.

    • Operate the analytical balance as per SOP.

    • Take the disc / SS bowl and place on the pan and tare it.

    • Select 20 capsules.

    • Weigh an intact capsule and record the weight.

    • Open the capsule without losing any part of the shell and remove the contents as completely as possible.

    • Weigh the empty capsule and record the weight.

    • The weight of the contents is the difference between the weighing.

    • Repeat the procedure with a further 19 capsules.

    • Determine the average weight.

    • Acceptance Criteria:

    • None capsule should deviates by percentage given below or as specified.

    • In critical case not more than two of the individual weights deviate from the average fill weight by more than the percentage given below and none deviates by more than twice that percentage.

Average fill Weight

Percentage Deviation

Less than 300 mg

10

300 mg or more

7.5

  • Calculation of % Variation:

                                 (Min. fill weight – Average fill weight)

   % Minimum Variation = ————————————————— x 100

                     Average fill weight

                                  (Max. fill weight – Average fill weight)

   % Maximum Variation = ————————————————— x 100

                       Average fill weight

  •  Uniformity of fill volume – In process Quality Control (IPQC):

    • Requirement:

    • Calibrated measuring cylinder (the capacity of cylinder shall be not more the three times of the volume to be measured)

    • Sample Quantity : Bottles equivalent to number of filling heads

    • Procedure:

    • Open one bottle and pour completely the contents into calibrated measuring cylinder and record the observation. Similarly measure the volume of the contents of the rest containers and record the observations

    • Acceptance criteria:

    • The average net volume of the contents of all the containers shall be not less than the claim.

    • The net volume of the contents of any single container shall comply the limits which are defined in respective BPR.

    • In process checks shall be done during packing of the OSD and Oral Liquid shall be done as per define in the respective BPR, like sealing, printing coding, leak test etc.

    • The leak test shall be done as per the SOP for Leak Test Apparatus

    • Any deviation observed during In process Quality Control (IPQC) checks, shall be communicated to concerned section in-charge, Head of Department and QA.

    • The deviations shall be handled following SOP for Incident / Deviation

4.0   Reference (S) – In Process Quality Control (IPQC) Tests :

    • Indian Pharmacopoeia, British Pharmacopoeia and United State Pharmacopoeia.

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