disintegration test

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DISINTEGRATION TESTS


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Table of Contents

Section Section Name

I Introduction of Disintegration test

2. Application and Uses

3 Advantages and disadvantage

4 General Principles involved in testing

5 Different Methods

6 Instrumentation (Models)

Disintegration

Tests


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Introduction of Disintegration Tests

For a drug to be absorbed from a solid dosage form after oral administration, it must first be in solution, and the first important step toward this condition is usually the break-up of the tablet; a process known as disintegration.

• It is a measure of the time required under a given set of conditions for a group of tablets to disintegrate into particles which will pass through a 10 mesh screen.

• The test is useful as a quality assurance tool for conventional dosage forms.

Disintegration Test


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This method is not applied for preparations exceeding 20.00 mm in diameter, for sustained release preparations, or for preparations which subject to the Dissolution Test.

• It is a method to determine the resistance or disintegration of solid preparations for internal use in the test fluids.

• Dosage forms: Tablets, tablet coated with suitable coating agents, pills, capsules, granules or enteric coated preparations.

Introduction of Disintegration Tests

Disintegration Test


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Applicationand Uses:

1.To find out the time it takes for a solid oral dosage form to completely disintegrate.• The time of disintegration is a measure of the quality

• Ex: Disintegration time – too

high• Tablet – too highly

compressed• Capsule shell gelatin

– not of pharmacopoeial quality


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4.This test is also a simple in-process control tool to ensure uniformity from batch to batch and among different tablets.

5.It is also an important test in the quality control of tablets and hard gelatin capsules.



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Advantages:

• This test is simple in concept and in practice.

• It is very useful in preformulation, optimisation and in quality control.

Advantages and disadvantages:


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Disadvantages:

• Disintegration test cannot be relied upon for the assurance of bioavailability.

Advantages and disadvantages:


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Principles Involved in Disintegration Apparatus

• Discs are used in the disintegration test to avoid the Floating of tablet when immersed in the medium ,so that equal disintegration occurs in all the tablets under testing.

Principles Involve


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Ex: Enteric coated ones the usual procedure is first we are dipping in HCl to mimic the gastric fluid medium and then we are using an alkaline medium to dissolve the enteric coated phalate layers mimicking the intestinal environment.

• The usual medium used is water (neutral) for most of the dosage forms;

• In some cases we are using acidic and basic medium case

Principles Involve


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The use of discs is to avoid floating of dosage units

ensuring uniform exposure of medium to all the surfaces of the dosage unit.

• In general the specification of temperature is not so important in case of solid dosage forms where as in case of semi-solid dosage forms being made of lipids temperature should be specified in-order to avoid melting of lipids.

Principles Involve


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Disintegration Test Methods

• The disintegration test for each dosage form is given in the pharmacopoeia. There are some general tests for typical types of dosage forms. However, the disintegration test prescribed in the individual monograph of a product is to be followed.

Methods or Procedures

If the monograph does not specify any specific test, the general test for the specific dosage form may be employed.


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1. Attach the basket-rack assembly to the bearing, immerse in fluid in a beaker, and adjust the apparatus so as to raise and lower the basket smoothly at a constant frequency of 29 to 32 cycles per minute through a distance of 53 to 57 mm.


General Procedure:


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2. At the lowest point of the downward stroke, the wire mesh must be 25 mm distant from the bottom of the beaker and the volume of the fluid in the beaker is such that, at the lowest point of the downward stroke, the top of the basket is on a level with the surface of the fluid. Maintain the temperature of the fluid at 37 ± 2oC during the test.


General Procedure:


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3. Place the Sample, except for granules, to be tested in each of the 6 tubes of the basket, immerse the basket in a suitable volume of test fluid, maintained in a beaker at the desired temperature, and operate the apparatus for the directed period of time.


General Procedure:


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4. At the end of that period, lift the basket gently from the fluid to permit the observation of the samples in the glass tubes. When it is directed to put auxiliary disks in the tubes, place a sample in each tube, then put the disk gently in each tube with the upper side up, and proceed as directed above. If the determination is difficult, the auxiliary disk may be omitted.


General Procedure:


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• Apply the test for Uncoated Tablets.

• Attach a removable wire cloth, which has a plain square weave with 1.8- to 2.2-mm mesh apertures and with a wire diameter of 0.60 to 0.655 mm, as described under Basket-Rack Assembly, to the surface of the upper plate of the basket-rack assembly.

Hard Gelatin CapsulesMethods or Procedures


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• Observe the capsules within the time limit specified in the individual monograph: all of the capsules have disintegrated except for fragments from the capsule shell.

Hard Gelatin CapsulesMethods or Procedures


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• Proceed as directed under Hard GelatinCapsules.

Soft Gelatin CapsulesMethods or Procedures


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• Place 1 tablet in each of the six tubes of the basket and operate the apparatus, using distilled water as meduim and maintained at 37oC the immersion fluid unless otherwise specified in the individual monograph.

• 15 minutes

Uncoated Tablets



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• At the end of the time limit specified in the monograph, lift the basket from the fluid, and observe the tablets: all of the tablets have disintegrated completely.

Uncoated TabletsMethods or Procedures


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• Apply the test for Uncoated Tablets, but the time of operation is 30 minutes.

Plain Coated TabletsMethods or Procedures


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• Place 1 tablet in each of the six tubes of the basket and, Suspend the assembly in a beaker with 0.1 M Hcl. Operate without discs for 2 hrs. (Unless otherwise stated in the monograph).

• Remove the set up from the liquid.

Delayed-Release (Enteric Coated) Tablets



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• Replace the liquid in beaker with mixed phosphate buffer of pH 6.8 and, Add a disc to each tube and operate the apparatus for further 1 hr.

• Remove the apparatus from the liquid. If no residue remains on the screen, then the six tablets are said to be completely disintegrated.




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• Operate the apparatus, using simulated intestinal fluid TS maintained at 37 C as the immersion fluid, for the time specified in the monograph.

• Lift the basket from the fluid, and observe the tablets: all of the tablets disintegrate completely.




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• After 4 hours, lift the basket from the fluid, and observe the tablets: all of the tablets have disintegrated.

Buccal TabletsMethods or Procedures


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• Observe the tablets within the time limit specified in the individual monograph: all of the tablets have disintegrated.

Sublingual TabletsMethods or Procedures


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• Place a pessary or a suppository on the lower perforated disc of the metal device.

• Insert the device into the cylinder and attach this to the sleeves.

• The same operation is repeated with further two pessaries or suppositories and metal devices and sleeves.

Pessaries and SuppositoriesMethods or Procedures


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• If specified, place each piece of apparatus in a vessel containing 4 liters of water at a temperature of 36-37 ºc, fitted with a slow stirrer and a means of holding the top of apparatus 90 mm below the surface of water. Alternatively, all the three pieces of apparatus may be placed together in a vessel containing 12 liters of water.

Pessaries and Suppositories Methods or Procedures


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• After each 10 min invert each apparatus without removing from the liquid.

• Disintegration is said to be completed when the moulded pessary or suppository:

• is completely dissolved• has dispersed into its component parts or

• remains on the surface (in the case of melted fatty substances)



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• sinks to the bottom(in the case of insoluble powders)

• dissolves (in the case of soluble components)

• Or may be distributed in one or more of these ways:

- has become soft with appreciable change in shape

- consisting of only a soft mass having no solid core which cannot be pressed with a glass rod.



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USP Specifications

Formulation United States Pharmacopoeia 2009

Hard Gelatin Capsules

Same as uncoated tablets. Use a circular cloth mesh of diameter 0.60-0.655mm & 1.8-2.2mm square mesh size. No palpable material to remain on the mesh.

Soft gelatin capsules

Same as uncoated tablets. Use a circular cloth mesh of diameter 0.60-0.655mm & 1.8-2.2mm square mesh size. No palpable material to remain on the mesh.


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USP Specifications


Uncoated tablets

Uses disintegration apparatus with specified liquid medium & for specified time as per monograph. If 1-2 fail, repeat for 12 different units. 16 out of 18 indicate test is affirmative.

Chewable tablets

Same as uncoated tablets. Uses disintegration apparatus with specified liquid medium & for 4 hours or as per monograph. If 1-2 fail, repeat for 12 different units. 16 out of 18 indicate test is affirmative.


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USP Specifications


Non-film coated tablets

Same as uncoated tablets. Uses disintegration apparatus with specified liquid medium & for specified time as per monograph. If 1-2 fail, repeat for 12 different units. 16 out of 18 indicate test is affirmative.

Film coated tablets

Same as uncoated tablets. Uses disintegration apparatus with specified liquid medium & for specified time as per monograph. If 1-2 fail, repeat for 12 different units. 16 out of 18 indicate test is affirmative.


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USP Specifications


Gastro resistant tablets (Enteric Coated)

Uses disintegration apparatus with stimulated gastric fluid TS at 37+-2OC for 1 hour, if there is no cracking or breaking of coat, continue with stimulated intestinal fluid at same temperature for specified time as per monograph. If 1-2 fail, repeat for 12 different units. 16 out of 18 indicate test is affirmative.


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USP Specifications


Buccal Tablets

If 1 or 2 tablets fail to disintegratecompletely, repeat the test on 12 additional tablets: not less than 16 ofthe total of 18 tablets tested disintegrate completely.

Sublingual Tablets

If 1 or 2 tablets fail to disintegrate completely, repeat the test on 12 additional tablets: notless than 16 of the total of 18 tablets tested disintegrate completely.


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USP Specifications


Suppositories Uses disintegration apparatus with water R or specified liquid medium & for 30 min. for suppositories with fatty base and for 60 min. for suppositories with water soluble base. If 1-2 fail, repeat for 12 different units. 16 out of 18 indicate test is affirmative.

Effervescent tablets

A total of 6 units tested Uses 200ml of water R at 15-25OC. Disintegrates within 5 min. or as per monograph. If 1-2 fail, repeat for 12 different units. 16 out of 18 indicate test is affirmative.


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USP Specifications


Modified release capsules

Disintegration test not applicable

Modified release tablets

Disintegration test not applicable


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It consists of:•Basket-rack assembly•Beaker (1 L capacity)•Thermostat arrangement Mechanical device (raising and lowering the basket)•Immersion fluid.

Apparatus for Tablets and Capsules:

Instrumentations:


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• Basket made of transparent polyvinyl or other plastic material

• It consists of six cylindrical glass tubes (length: 77.5+/- 2.5 cm long, internal diameter: 20.7 - 23 mm, wall thickness: 1.0-2.8 mm).

Basket- rack assembly Instrumentations:


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• The tubes are held in position by two superimposed transparent plastic plates, perforated by six holes having the same diameters as the tubes. (Diameter: 8.8-9.2mm thickness: 5-7mm)



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• To the underside of the lower plastic plate is a woven stainless steel wire cloth with a plain square weave with 1.8-2.2mm mesh apparatus and with a diameter of 0.60-0.665mm.



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• The upper plate is covered with a six holed stainless steel disc, each about 24+/- 2 mm in diameter, which fits over the tubes and holds them between the plastic plates.



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• A cylindrical disc made of transparent plastic is provided for each tube, (Diameter: 20.7+/- 0.15 mm; thickness: 9.5+/- 0.15; relative density: 1.18- 1.20).

DiscInstrumentations:


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• In each disc there are five holes (diameter of 2mm) one in the center and four surrounded equidistantly on a circle of radius 6 mm from the centre are provided.



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• Four equally trapezoidal shaped grooves are cut in the lateral surface of the disc they are 9.5 mm wide and 2.25mm deep at the lower surface 1.6mm square.



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Disc Instrumentations:

disks with metal

contact ring and metal needles

Disks with

ring (no needle)


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Disc Instrumentations:

disks and metal contact plate

StandardDisintegra

tion USP/EP Disks


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Medium Instrumentations:• The assembly is to be suspended in a 1L beaker.

• The volume of the liquid is such that the wire mesh at its highest point is atleast 25mm below the surface of the liquid, and its lowest point is atleast 25 mm above the bottom of the beaker; one must make sure that the top of the basket rack assembly shouldn’t be submerged.


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Heating DeviceInstrumentations:

• There is a thermostat arrangement for heating the liquid and maintaining the temperature at

35 and 39oC


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Instrumentations:

Basket-rack assembly

Individual glasstube

Disc

Sieve meshes

Mechanical Device

Heating Device


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Instrumentations:Diagram of Assembly Apparatus

Basket-rack Assembly

Cylinder in down position

Basket-rack Assembly

Level f Liquid at 37oC2.5L of Medium

Device for Raising and

lowering Basket-Rack

Assembly

Support


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Diagram of Glass Tube, Plastic Disk, and Plunger

12 Holes

Wire Rod (3.2 cm x 9 cm)

6 Holes

2 mm Wall

Inside diameter of NLT 21.0mm and NMT 22.5mm

Disk

Screen


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Apparatus for Pessariesand Suppositories

Instrumentations:

• A transparent sleeve made of glass or plastic. (Height: 60mm, Internal Diameter: 52 mm; appropriate wall thickness).

• A metal device consisting of two stainless discs; each of which contains 39 holes, each 4 mm in diameter.


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Apparatus for Pessariesand Suppositories

Instrumentations:

• The discs are separated by a distance of 30 mm.

• The metal device is attached to the outer sleeve by means of three equally shaped hooks; also the diameter of disc is closely similar to the internal diameter of the sleeve.


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Suppositories Disintegration Tester

Instrumentations:

• 3 independent test stations perform tests simultaneously

• All test cylinders turn 180 o C ( 10 mins)

• Test cylinders turning interval can be programmed from 1 min to 99 min

• Removable thermostat can be programmed to maintain temperature between 30 o C to 50 o C (+/- 0.5 o C) in the bath


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Suppository Disintegration TestPTS-3E

Instrumentations:

• According to the Pharmacopoeia monograph 3 samples are tested at the same time.

• The total testing period can be pre-set within a range of 1 minute to 10 hours.

• When used to test suppositories the sample baskets will turn automatically each 10 minutes through 180 degrees as specified in the relevant monograph.


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Instrumentations:

• Automatic rotation through 180 degrees when suppositories are tested

• Selectable cycling time for 1 - 10 Min.

• Programmable testing time for 1 min. to 10 hours

• Digital display of elapsed testing time

• Recall pre-set total time Basket sample Holder Complete


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Instrumentations:

• Built-in circulation thermostat, adjustable for 30°C - 40°C +/- 0.5°C accuracy

• Simultaneous test of 3 samples possible as per EP monograph

• Heating system protected against grease intrusion

• Water bath volume > 12 L Basket Including Suppository


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Single Basket Disintegration Apparatus

Instrumentations:

• The cylinder moves up and down 30 to 32 cycles/min.

• In one liter beaker filled with distilled water, maintained at 37 c + 2 c by thermostatically controlled hot plate

• complete with beaker of `borosil` to work on 220/230 volts, with wire and plug, ready to switch on


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Double Basket Disintegration Apparatus

Instrumentations:

• Double basket unit , equipped with water bath designed to conduct disintegration tests as per new IP & USP standards.

• Temperature of the water bath is precisely controlled by sensitive thermostat.


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Triple Basket Disintegration Apparatus

Instrumentations:

• It is suitable for tablet and capsule disintegration testing as per USP<701/2040> and EP<2.9.1/2.9.1.2>

• Operates 3 Baskets which are connected to a central stroke arm


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Automatic Tablet Disintegration Testing

Instrumentations:

• Automatic measuring of tablet thickness

• Graphical display of disintegration characteristics over time (curve)

• Precise inductive measuring technology

• Corrosion-free• Self-centering magnetic baskets

• Fast and easy cleaning• 100% USP and EP compliant design


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Automatic tablet

disintegration tester with

single testing station

Instrumentations:


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Automatic tablet

disintegration tester with two independent

testing stations

Instrumentations:


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Automatic tablet

disintegration tester with three

independent testing stations

Instrumentations:


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Automatic tablet

disintegration tester with four

independent testing stations

Instrumentations:


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Manual Disintegration Testing

Instrumentations:

• Pharmacopoeia compliance and qualification

• Simple operation• Quick-release basket design

• One-piece water bath• Independent heater / circulator

• Low liquid-level sensor

• Acoustic signal at end of test

• Constant monitoring of time and temperature(displayed on LCD screen)


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Manual Disintegration

Testing

Instrumentations:

ONE TEST STATION


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Testing

Instrumentations:

TWO TEST STATION


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Testing

Instrumentations:

THREE TEST STATION


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Thank you


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