Formulation,

Challenges and
Coating of
Tablets

Group no. : 91 - 100

1
An ideal tablet should be free from any visual defect or functional defect. The
advancements and innovations in tablet manufacture have not decreased the
problems, often encountered in the production, instead have increased the
problems, mainly because of the complexities of tablet presses; and/or the
greater demands of quality.

An industrial pharmacist usually encounters number of problems during

manufacturing. Majority of visual defects are due to inadequate fines or
inadequate moisture in the granules ready for compression or due to faulty
machine setting. Functional defects are due to faulty formulation. Solving
many of the manufacturing problems requires an in–depth knowledge of
granulation processing and tablet presses, and is acquired only through an
exhaustive study and a rich experience.

Here, we will discuss the imperfections found in tablets along–with their

causes and related remedies. The imperfections are known as: ‘VISUAL
DEFECTS’ and they are either related to imperfections in any one or more of
the following factors:

I. Tableting Process

II. Excipient

III. Machine

The defects related to Tableting Process are as follows:

1) CAPPING: It is due air-entrapment in the granular material.

2) LAMINATION: It is due air-entrapment in the granular material.

3) CRACKING: It is due to rapid expansion of tablets when deep concave

punches are used.

The defects related to Excipient are as follows:

4) CHIPPING: It is due to very dry granules

5) STICKING

6) PICKING

7) BINDING

2
The defect related to more than one factor:
8) MOTTLING: It is either due to any one or more of these factors: Due to a
coloured drug, which has different colour than the rest of the granular
material? (Excipient- related); improper mixing of granular material (Process-
related); dirt in the granular material or on punch faces; oil spots by using
oily lubricant.

The defect related to Machine:

9) DOUBLE IMPRESSION: It is due to free rotation of the punches, which have
some engraving on the punch faces.

Further, in this section, each problem is described along-with its causes and
remedies which may be related to either of formulation (granulation) or of
machine (dies, punches and entire tablet press).

1 - Capping
Definition: ‘Capping’ is the term used, when the upper or lower segment of
the tablet separates horizontally, either partially or completely from the main
body of a tablet and comes off as a cap, during ejection from the tablet press,
or during subsequent handling.

Reason: Capping is usually due to the air–entrapment in a compact during

compression, and subsequent expansion of tablet on ejection of a tablet from
a die.

THE CAUSES AND REMEDIES OF CAPPING RELATED TO ‘FORMULATION’

(GRANULATION)

Sr.
CAUSES REMEDIES
No.
Large amount of fines in the Remove some or all fines through 100 to
1.
granulation 200 mesh screen
Too dry or very low moisture Moisten the granules suitably. Add
2. content (leading to loss of hygroscopic substance e.g.: sorbitol,
proper binding action). methyl- cellulose or PEG-4000.
Not thoroughly dried
3. Dry the granules properly.
granules.
Increasing the amount of binder OR
Insufficient amount of binder
4. Adding dry binder such as pre-gelatinized
or improper binder.
starch, gum acacia, powdered sorbitol, PVP,
hydrophilic silica or powdered sugar.

3
 Insufficient or improper Increase the amount of lubricant or change
5.
lubricant. the type of lubricant.
Granular mass too cold to
6. Compress at room temperature.
compress firm.

THE CAUSES AND REMEDIES OF CAPPING RELATED TO ‘MACHINE’

(DIES, PUNCHES AND TABLET PRESS)

Sr. CAUSES REMEDIES

No.
Polish dies properly. Investigate other
1. Poorly finished dies
steels or other materials.
Deep concave punches or beveled-
2. Use flat punches.
edge faces of punches.
Lower punch remains below the Make proper setting of lower punch
3.
face of die during ejection. during ejection.
Incorrect adjustment of sweep-off Adjust sweep-off blade correctly to
4.
blade. facilitate proper ejection.
Reduce speed of turret (Increase
5. High turret speed.
dwell time).

2 - Lamination / Laminating
Definition: ‘Lamination’ is the separation of a tablet into two or more distinct
horizontal layers.

Reason: Air–entrapment during compression and subsequent release on

ejection.

The condition is exaggerated by higher speed of turret.

THE CAUSES AND REMEDIES OF LAMINATION RELATED TO

FORMULATION (GRANULATION)

Sr. CAUSES REMEDIES

No.
Oily or waxy materials in Modify mixing process. Add adsorbent
1.
granules or absorbent.
Too much of hydrophobic Use a less amount of lubricant or
2. lubricant e.g.: Magnesium- change the type of lubricant.
stearate.

4
 The Causes and Remedies of Lamination related to MACHINE (Dies,
Punches and Tablet Press)

Sr. CAUSES REMEDIES</ b>

No.
Rapid relaxation of the peripheral Use tapered dies, i.e. upper part of the
1. regions of a tablet, on ejection die bore has an outward taper of 3° to
from a die. 5°.
Use pre-compression step. Reduce
2. Rapid decompression turret speed and reduce the final
compression pressure.

3 - Chipping
Definition: ‘Chipping’ is defined as the breaking of tablet edges, while the
tablet leaves the press or during subsequent handling and coating
operations.

Reason: Incorrect machine settings, specially mis-set ejection take-off.

THE CAUSES AND REMEDIES OF CHIPPING RELATED TO FORMULATION

(GRANULATION) ARE AS FOLLOWS

Sr. CAUSES REMEDIES

No.
Dry the granules properly or increase
1. Sticking on punch faces
lubrication.
Moisten the granules to plasticize. Add
2. Too dry granules.
hygroscopic substances.
Too much binding causes
3. Optimize binding, or use dry binders.
chipping at bottom.

THE CAUSES AND REMEDIES OF CHIPPING RELATED TO MACHINE

(DIES, PUNCHES AND TABLET PRESS)

Sr. CAUSES REMEDIES

No.
Groove of die worn at compression Polish to open end, reverse or
1.
point. replace the die.
Barreled die (center of the die
2. Polish the die to make it cylindrical
wider than ends)
Edge of punch face turned
3. Polish the punch edges
inside/inward.
4. Concavity too deep to compress Reduce concavity of punch faces. Use
5
 properly. flat punches.

4 - Cracking
Definition: Small, fine cracks observed on the upper and lower central
surface of tablets, or very rarely on the sidewall are referred to as ‘Cracks’.

Reason: It is observed as a result of rapid expansion of tablets, especially

when deep concave punches are used.
THE CAUSES AND REMEDIES OF CRACKING RELATED TO
FORMULATION (GRANULATION)

Sr. CAUSES REMEDIES

No.
Large size of Reduce granule size. Add fines.
1.
granules.
Moisten the granules properly and add
2. Too dry granules.
proper amount of binder.
3. Tablets expand. Improve granulation. Add dry binders.
Granulation too Compress at room temperature.
4.
cold.

THE CAUSES AND REMEDIES OF CRACKING RELATED TO MACHINE

(DIES, PUNCHES AND TABLET PRESS)

Sr. CAUSES REMEDIES

No.
Tablet expands on ejection due to air
1. Use tapered die.
entrapment.
Deep concavities cause cracking while
Use special take-
2.
off.
removing tablets

5 - Sticking / Filming
Definition: ‘Sticking’ refers to the tablet material adhering to the die wall.

Filming is a slow form of sticking and is largely due to excess moisture in the
granulation.

Reason: Improperly dried or improperly lubricated granules.

6
THE CAUSES AND REMEDIES OF STICKING RELATED TO FORMULATION
(GRANULATION)

Sr. CAUSES REMEDIES

No.
Granules not dried Dry the granules properly. Make moisture
1.
properly. analysis to determine limits.
Too little or improper
2. Increase or change lubricant.
lubrication.
Reduce the amount of binder or use a different
3. Too much binder
type of binder.
Hygroscopic granular Modify granulation and compress under
4.
material. controlled humidity.
5. Oily or way materials Modify mixing process. Add an absorbent.
Too soft or weak Optimize the amount of binder and granulation
6.
granules. technique.

THE CAUSES AND REMEDIES OF STICKING RELATED TO MACHINE

(DIES, PUNCHES AND TABLET PRESS)

Sr. CAUSES REMEDIES

No.
Concavity too deep for Reduce concavity to
1.
granulation. optimum.
2. Too little pressure. Increase pressure.
3. Compressing too fast. Reduce speed.

6 - Picking
Definition: ‘Picking’ is the term used when a small amount of material from a
tablet is sticking to and being removed off from the tablet-surface by a punch
face.

The problem is more prevalent on the upper punch faces than on the lower
ones. The problem worsens, if tablets are repeatedly manufactured in this
station of tooling because of the more and more material getting added to
the already stuck material on the punch face.

Reason: Picking is of particular concern when punch tips have engraving or

embossing letters, as well as the granular material is improperly dried.

THE CAUSES AND REMEDIES OF PICKING RELATED TO FORMULATION

(GRANULATION)
7
Sr. CAUSES REMEDIES
No.
Dry properly the granules, determine
1. Excessive moisture in granules.
optimum limit.
Increase lubrication; use colloidal silica
2. Too little or improper lubrication. as a ‘polishing agent’, so that material
does not cling to punch faces.
Low melting point substances,
Add high melting-point materials. Use
3. may soften from the heat of
high meting point lubricants.
compression and lead to picking.
Low melting point medicament in Refrigerate granules and the entire
4.
high concentration. tablet press.
Too warm granules when Compress at room temperature. Cool
5.
compressing. sufficiently before compression.
Reduce the amount of binder, change
6. Too much amount of binder.
the type or use dry binders.

THE CAUSES AND REMEDIES OF PICKING RELATED TO MACHINE (DIES,

PUNCHES AND TABLET PRESS)

Sr. CAUSES REMEDIES

No.
1. Rough or scratched punch faces. Polish faces to high luster.
Design lettering as large as possible.
Embossing or engraving letters on
2. punch faces such as B, A, O, R, P, Plate the punch faces with chromium
Q, G. to produce a smooth and non-adherent
face.
3. Bevels or dividing lines too deep. Reduce depths and sharpness.
Pressure applied is not enough;
4. Increase pressure to optimum.
too soft tablets.

7 - Binding
Definition: ‘Binding’ in the die, is the term used when the tablets adhere,
seize or tear in the die. A film is formed in the die and ejection of tablet is
hindered. With excessive binding, the tablet sides are cracked and it may
crumble apart.

Reason: Binding is usually due to excessive amount of moisture in granules,

lack of lubrication and/or use of worn dies.

THE CAUSES AND REMEDIES OF BINDING RELATED TO FORMULATION

(GRANULATION)
8
Sr. CAUSES REMEDIES
No.
Too moist granules and
1. Dry the granules properly.
extrudes around lower punch.
Insufficient or improper Increase the amount of lubricant or use a
2.
lubricant. more effective lubricant.
Reduce granular size, add more fines, and
3. Too coarse granules.
increase the quantity of lubricant.
Too hard granules for the
4. Modify granulation. Reduce granular size.
lubricant to be effective.
If coarse granules, reduce its size.
Granular material very
5.
abrasive and cutting into dies.
Use wear-resistant dies.
Reduce temperature.
Granular material too warm,
6.
sticks to the die.
Increase clearance if it is extruding.

THE CAUSES AND REMEDIES OF BINDING RELATED TO MACHINE (DIES,

PUNCHES AND TABLET PRESS)

Sr. CAUSES REMEDIES

No.
1. Poorly finished dies. Polish the dies properly.
Rough dies due to Investigate other steels or other materials or
2.
abrasion, corrosion. modify granulation.
Rework to proper size.
Undersized dies. Too little
3.
clearance.
Increase clearance.
Reduce pressure. OR
Too much pressure in the
4.
tablet press.
Modify granulation.

8 - Mottling
Definition: ‘Mottling’ is the term used to describe an unequal distribution of
colour on a tablet, with light or dark spots standing out in an otherwise
uniform surface.

Reason: One cause of mottling may be a coloured drug, whose colour differs
from the colour of excipients used for granulation of a tablet.

THE CAUSES AND REMEDIES OF MOTTLING

9
Sr. CAUSES REMEDIES
No.
A coloured drug used
along with colourless or
1. Use appropriate colourants.
white-coloured
excipients.
Change the solvent system,

A dye migrates to the Change the binder,

2. surface of granulation
while drying. Reduce drying temperature and

Use a smaller particle size.

Improperly mixed dye,
Mix properly and reduce size if it is of a larger
3. especially during ‘Direct
size to prevent segregation.
Compression’.
Incorporate dry colour additive during powder
Improper mixing of a blending step, then add fine powdered
4.
coloured binder solution. adhesives such as acacia and tragacanth and
mix well and finally add granulating liquid.

9 - Double impression
Definition: ‘Double Impression’ involves only those punches, which have a
monogram or other engraving on them.

Reason: At the moment of compression, the tablet receives the imprint of

the punch. Now, on some machines, the lower punch freely drops and travels
uncontrolled for a short distance before riding up the ejection cam to push
the tablet out of the die, now during this free travel, the punch rotates and at
this point, the punch may make a new impression on the bottom of the
tablet, resulting in ‘Double Impression’.

If the upper punch is uncontrolled, it can rotate during the short travel to the
final compression stage and create a double impression.

THE CAUSES AND REMEDIES OF DOUBLE IMPRESSION

Sr. CAUSE REMEDIES

No.
-Use keying in tooling, i.e. inset a key
alongside of the punch, so that it fits the
Free rotation of either upper
punch and prevents punch rotation.
1. punch or lower punch during
ejection of a tablet.
-Newer presses have anti-turning devices,
which prevent punch rotation.
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The last steps is tablet formulation is Coating of tablets , before coating the
tablet we have to know the reason for coating , types of coating and the
problems we meet when coating the tablet.

* Reasons for Coating:

1- Protection of the drug from the surrounding (environment) (air, light
and moisture) and thus improve stability.

2- Modifying drug release, as in enteric coating and extended-release

formulation.

3- Masking unpleasant taste or odor of the drug.

4- Improving product appearance and helping in brand identification.

5- Facilitating rapid identification by the manufacturer, the pharmacist

and the patient (mostly colored).

6- Increasing the mechanical strength of the product.

7- Masking batch differences in the appearance of raw materials.

*Types of coating processes:

Three main types are used in the pharmaceutical industry today;

1- Film coating

2- Sugar coating

3- Compression coating

4- Gelatin coating (not common)

1- Film coating (the most popular today)

It involves the deposition, usually by spraying method, of a thin
uniform film of a polymer formulation surrounding a tablet.

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* Types of film coating:

1- Immediate release (non functional) film coating:

They do not affect the biopharmaceutical properties of the tablet. They

are readily soluble in water.

2- Modified release (functional) film coating:

They allow the drug to be delivered in a specific manner; i.e. they

affect drug release behavior. Modified release film coatings are sub
classified into;

a - Delayed release coating (enteric coating):

Only soluble in water at pH ≥5 6

Intended to protect the drug from gastric acidic pH (for acid

labiledrugs)

Used for colonic drug delivery systems

b- Extended release coating:

Mostly water insoluble.

Designed to ensure consistent drug release manner over a long period

of time (6 - 12 hr) and thus decreasing dosing regimen and improving
patient compliance.

* Film coating formulation (Composition of the coating liquid):

1- Polymer 2- Plasticizer

3- Colorants 4- Solvent
(vehicle)

1- Polymer

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A film former capable of producing smooth thin films reproducible
under the prescribed coating conditions.

-- Immediate-release coating polymers

a- Cellulose derivatives:

The most widely used of cellulosic polymers is HPMC

-Advantages:

•it is readily soluble in aqueous media

• forms film with good mechanical properties (strength, flexibility and

adhesion to the tablet

• easy application of the coat

Other examples are MC & HPC

b- Vinyl derivatives:

PVP, it has a limited use in coating because of its inherent tackiness.

A copolymer of PVP and vinyl acetate forms better films.

-- Modified-release coating polymers

1- Extended-release coating polymers

They are dissolved in organic solvent or dispersed in aqueous medium

a- Cellulose derivatives:

Highly substituted cellulosic ether, thus rendering the polymer water

insoluble, e.g. Ethyl cellulose (EC).

2- Enteric-coating polymers

a- Methacrylic acid copolymers:

The presence of carboxylic acid groups renders this class to be

insoluble in water at low pH (stomach) but gradually becomes soluble
as the pH rises towards neutrality (upper part of the small intestine).

b- Phthalate esters:

13
e.g. Cellulose acetate phthalate (CAP).

2- Plasticizer

Plasticizer: Affords flexibility and elasticity to the coat and thus provide
durability.

Examples; Polyethylene glycol (PEG), Polypropylene glycol and coconut

oil.

3- Colorants

Provides an elegant appearance. Ex. Iron oxide pigment, Titanium

dioxide and Aluminum lakes.

4- Solvent (vehicle)

Volatile organic solvents may be used to allow good spreadability of

the coat components over the tablet and allowing rapid evaporation,
but they are expensive and show environmental hazards and solvent
residue in the formulation must be investigated (certain limit).
Aqueous vehicles are safer, but they show slower evaporation and may
affect drug stability.

2- Sugar - coating of tablets (traditional):

- It involves successive application of sucrose- based coating
formulations to tablet cores, in suitable coating equipment. Water
evaporates from the syrup leaving a thick sugar layer around each
tablet. Sugar coats are often shiny and highly colored.

- Steps for sugar-coating process: (6 steps, so that it is time

consuming)

1- Sealing of the tablet cores

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2- Sub coating

3- Smoothing

4- Coloring

5- Polishing

6- Printing

1- Sealing (Water proofing):

- This involved the application of one or more coats of a waterproofing

substance in the form of alcoholic spray, such as pharmaceutical
Shellac (traditionally) or synthetic polymers, such as CAP.

(N.B. unless a modified release feature needs to be introduced, the

amount of the sealing coat applied should be carefully calculated so
that there is no negative effect on the drug release characteristics in
case of immediate release product.)

- Advantages:

a- Sugar- coatings are aqueous formulations which allow water to

penetrate directly into the tablet core and thus potentially affecting
product stability and possibly causing premature tablet disintegration.

b- Application of many coats of partially or completely water insoluble

polymers in this step, enables sugar coated product to exhibit modified
release pattern (extended-release or delayed "enteric"-release
characteristics).

2- Sub coating

- Large quantities of sugar coatings are usually applied to the tablet

core (typically increasing the tablet weight by 50-100%) in order to
round off the tablet edge. Much of this material build up occurs during
this stage and is achieved by adding a bulking agent such as Calcium
carbonate, to the sucrose solution.

- Anti-adherents e.g. Talc may be added after partial drying to prevent

sticking of the tablets together.

15
N.B. These procedures may be repeated till the desired shape and size
are obtained.

3- Smoothing

The sub coating stage results in tablets with rough surfaces. To

facilitate the color application (which requires a smooth surface),
subcoated tablets are smoothed out by a thick sucrose syrup coating.

4- Coloring

Color coatings usually consist of thin sucrose syrup containing the

requisite coloring materials. (Water-soluble dyes or water-insoluble
pigments may be used)

N.B. This step must be done into a clean pan deprived of any residues
from the previous operations.

5- Polishing

After the coloring step, the tablet surfaces tend to be smooth but
somewhat dull in appearance. To achieve glossy finish, final stage
involving application of waxes (beeswax or carnuba wax) is employed.

6- Printing

Different tablets could be identified by manufacturer’s logo, product

name, dosage strength or other appropriate code. For sugar coated
tablets, such identification could be only achieved by printing process
using special edible inks.

3- Compression-coating of tablets
Although less popular, it gained increased interest in the recent years
for creating modified released products. It involves the compaction of
granular materials around a preformed tablet core using specially
designed tableting equipment. Compression coating is a dry process.

16
(After tab. Core manufacture, it is transferred (centrally positioned) to
another slightly larger die that is partially filled with the coating
powder. More coating powder is filled on the top of the core and
compressed again resulting in tablet within tablet)

Mechanically, it is a complex process, as the tablet may be tilted when

transferred to the second die cavity.

-Advantages:

Mostly, the coat is water-soluble and disintegrates easily after

swallowing, in order to achieve immediate-release product}.

1- Traditionally, to separate incompatible materials (One in the core

and the other in the coat). There is an interface between the two layers
and thus compromise product stability. It is possible to apply an inert
placebo coating layer first, to separate the core from the final coat
more effectively.

2- May be used to create modified-release products.

4- Gelatin-coated tablets
A recent innovation is the gelatin coated tablets. The innovator
product, the gelcap, is a capsule shaped compressed tablet coated
with gelatin layer.

17
- Advantages:

1- This allows the coated product to be about one-third smaller than a

capsule filled with an equivalent amount of powder.

2- The gelatin coating facilitates swallowing.

3- Gelatin coated tablets are more tamper evident than unsealed

capsule.

*Coating defects:
Here is a list of common defects associated with coated tablets and
some likely causes.

1- Picking and sticking

This is when the coating removes a piece of the tablet from the core. It
is caused by over-wetting the tablets, by under-drying, or by poor
tablet quality.

2- Bridging

This occurs when the coating fills in the lettering or logo on the tablet
and is typically caused by improper application of the solution, poor
design of the tablet embossing, high coating viscosity, high percentage
of solids in the solution, or improper atomization pressure.

18
3- Capping

This is when the tablet separates in laminar fashion. The problem

stems from improper tablet compression, but it may not reveal itself
until you start coating. Good operating the coating system, however,
can exacerbate the problem. Be careful not to over-dry the tablets in
the preheating stage. That can make the tablets brittle and promote
capping.

4- Erosion

This can be the result of soft tablets, an over-wetted tablet surface,

inadequate drying, or lack of tablet surface strength.

5- Twinning

This is the term for two tablets that stick together; and it’s a common
problem with capsule-shaped tablets. Assuming you don’t wish to
change the tablet shape, you can solve this problem by balancing the
pan speed and spray rate. Try reducing the spray rate or increasing
the pan speed. In some cases, it is necessary to modify the design of &
Capsules the tooling by very slightly changing the radius. The change
is almost impossible to see, but it prevents the twinning problem.

6- Peeling and frosting

This is a defect where the coating peels away from the tablet surface
in a sheet. Peeling indicates that the coating solution did not lock into
the tablet surface. This could be due to a defect in the coating solution,
over-wetting, or high moisture content in the tablet core.

7- Chipping

This is the result of high pan speed, a friable tablet core, or a coating
solution that lacks a good plasticizer.

8- Mottled color

This can happen when the coating solution is improperly prepared, the
actual spray rate differs from the target rate, the tablet cores are cold,
or the drying rate is out of spec.

9- Orange peel

19
This refers to a coating texture that resembles the surface of an
orange. It is usually the result of high atomization pressure in
combination with spray rates that are too high.

INDEX
20
The defects related to Tableting Process
2

The defects related to Excipient

2

The defect related to more than one factor

3

The defect related to Machine

3

1 – Capping
3

2 - Lamination
4

3 – Chipping
5

4 – Cracking
6

5 - Sticking / Filming
6

6 – Picking
7

7 – Binding
8

8 – Mottling
9

9 - Double impression
10

Reasons for Coating

11

Types of coating processes

11

Coating defects
18
21