Technical Information

Kollicoat IR

February 2013
Supersedes issue dated February 2010
03_030724e-11/Page 1 of 14
WF-No.: 121971

= Registered trademark of BASF

 olyvinyl alcohol-polyethylene glycol graft copolymer for instant-release

P
coatings and quick-dissolving formulations

03_030724e-11 February 2013

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Kollicoat IR

Contents
Page

1. Introduction

1.1 General

1.2 Structural formula

1.3 Physical form

2. Specification and properties

2.1 Chemical nature

2.2 Physicochemical properties

2.3 Specification

2.4 Regulatory status

2.5 Properties of aqueous solutions

2.6 Film properties

3. Application and processing

3.1 Applications

3.2 Processing notes

4. Typical formulations

4.1 Instant release coating Propranolol film-coated tablets

4.2 Instant release coating Caffeine tablets

4.3 Wet binding Acetaminophen instant granules

10

4.4 Drug layering Layering of Riboflavin onto pellets

10

4.5 Pore former in sustained release coating

Propranolol single unit drug delivery system

11

4.6 Wet binding Using GranuLac 200

12

5. Storage conditions

14

6. Stability

14

7. Toxicology

14

8. PRD-No.

14

9. Packaging

14

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Kollicoat IR

1. Introduction
1.1 General

Kollicoat IR is a polyvinyl alcohol-polyethylene glycol graft copolymer that is freely

soluble in water. It is used mainly for the production of instant-release coatings for
tablets.

1.2 Structural formula

O
O

HO
n

n-x

OH

OH

1.3 Physical form

Kollicoat IR is a white to faintly yellow free-flowing powder.

2. Specification and properties

2.1 Chemical nature

The polymer consists of 75% polyvinyl alcohol units and 25% polyethylene glycol
units. The product also contains approx. 0.3% colloidal silica to improve its flow
properties.

2.2 Physicochemical properties

As a result of its structure, the polymer dissolves very readily in acidic, neutral
and alkaline aqueous media. Such aqueous solutions have a comparatively low
viscosity.

Molecular weight

Approx. 45.000 Daltons

Solubility

Solutions of Kollicoat IR with concentrations of up to 40% can be prepared in

water and aqueous systems, e.g. weak acids or alkalis. Solutions of up to 25%
can be prepared in a 1:1 ethanol-water mixture. Due to colloidal silica, aqueous
solutions of Kollicoat IR are slightly turbid. Its solubility in non-polar solvents is low,
and it can only be dispersed in these.

Film formation

An aqueous solution of Kollicoat IR is cast on a smooth surface. When the water

has evaporated, a clear colourless flexible film remains (see 2.4, Film properties).

2.3 Specification

See separate document: Standard Specification (not for regulatory purposes)

available via BASFs WorldAccount: https://worldaccount.basf.com (registered
access).

Analytical procedures (non compendial methods) are supplied upon request.

03_030724e-11 February 2013

2.4 Regulatory status

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Kollicoat IR

Kollicoat IR is registered around the world in medicinal products in all relevant regions,
including Europe, Japan and the USA. Comprehensive safety documentation is
available, including non-clinical studies.
Kollicoat IR has received self-affirmed GRAS status as of January 2013. This
status allows its formulation into products for the US dietary supplements market.

Monographs & Registrations

Ph.Eur.

Macrogol poly(vinyl alcohol) graft polymer

USP/NF

Ethylene glycol and vinyl alcohol graft copolymer

PMDA (Japan)

Approved

JPE Listed
IIG listing

FDA approval received Jan 2012, database listing expected

2.5 Properties of aqueous solutions

Viscosity

Though the viscosity of aqueous solutions of Kollicoat IR increases with the polymer
concentration, yet at a much lower level than that of equivalent solutions, for
instance, cellulose derivatives.

Log. dynamic viscosity [mPas]

1.OE+04

1.OE+03

1.OE+02

1.OE+01

1.OE+00

10
15
20
25
Polymer concentration in water [%]

Kollicoat IR

HPMC 3 mPas

Kollicoat Protect
PVA

HPMC 6 mPas

30

Viscosity of aqueous Kollicoat IR solutions as a function of polymer concentration

Surface activity

Kollicoat IR reduces the surface tension of water. This makes aqueous solutions
easy to spray, and the spray droplets exhibit good wetting behavior on the tablet
surface.

03_030724e-11 February 2013

Kollicoat IR

Kollicoat IR forms clear colourless films that are enormously flexible and dissolve
very rapidly in water. Kollicoat IR films are not tacky, have a high pigment binding
capacity and can readily be p
rinted. The reduction of the surface tension is specifically
important for the processing in drug layering.
Kollicoat IR has a much higher elongation at break value than cellulose derivatives.
70
60
50
Strain [N/mm2]

2.6 Film properties

Page 5 of 14

40
30
20
10
0

50

100
150
Elongation [%]

200

Kollicoat IR

HPMC 3 mPas

Kollicoat Protect
PVA

HPMC 6 mPas

Elongation at break of various instant release polymers (54% r.h.)

250

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Kollicoat IR

3. Application and processing

3.1 Applications

Kollicoat IR can be used for all applications for which a water-soluble flexible polymer
is required.

Instant release coating

Wet binder
Pore former in sustained-release coatings
Film former in sprays and transdermal therapeutic systems
Suspension and emulsion stabiliser
Protective colloid
Film former in oral wafers

The special advantages of Kollicoat IR lie in its enormous flexibility, low viscosity
and rapid rate of dissolution.
Kollicoat IR solutions for spraying onto tablets can be applied with a high solids
content, which greatly reduces the coating time and minimizes costs.
3.2 Processing notes

Because of the high elasticity of Kollicoat IR films, it is not necessary to add

a plasticizer.
A spray suspension is best prepared as follows:
Dissolve Kollicoat IR in water and stir in the previously homogenized pigment
suspension. The other water-soluble ingredients can be dissolved together with
the Kollicoat IR. The type and speed of the stirrer s hould be set such that little or
no foam is produced.
As spray suspensions of Kollicoat IR have a lower viscosity than those of other
instant release polymers, they can have a much higher concentration. This g
reatly
shortens the spraying and processing time in the manufacture of film-coated tablets.
Polymer concentrations of 1525% can be used, giving a total solids concentration
of 2035%, depending on the quantity of pigments.
Since Kollicoat IR has surfactant properties and can act as a protective colloid,
it prevents the aggregation of the pigment particles and ensures that the pigment
is evenly distributed over the tablet core.
The great elasticity of Kollicoat IR e
nsures that it does not crack on the tablets when
they are exposed to different humidity conditions in storage, even when the cores
contain high amounts of disintegrant or powerful swelling a
gents such as HPMC,
xanthan or alginate which are frequently used in sustained release tablets.
The coating can be applied in all the usual coaters, e.g. side-vented drum coaters,
fluidised bed coaters, solid wall coaters, and coating pans under the usual condi
tions for aqueous solutions.
The following conditions have been used successfully in numerous trials:
Inlet air temperature:
Outlet air temperature:
Atomizing pressure:

5080 C
3050 C
1.56 bar

The product can very easily be cleaned off equipment with warm or cold water.

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Kollicoat IR

4. Typical formulations
4.1 Instant release coating Propranolol film-coated tablets
Composition of the tablets

40 mg propranolol HCl; 97.5 mg Ludipress; 12.5 mg Kollidon VA 64;

97.5 mg MCC PH 102; 2.5 mg magnesium stearate

Composition of the spray

suspension

The formulation is designed for 250 kg of tablets (tablet weight 250 mg;
diameter 9 mm)
Weight [g]

Proportion [%]

Polymer solution
Kollicoat IR

6.080

16.0

24.320

64.0

Talc

1.710

4.5

Titanium dioxide

1.140

3.0

570

1.5

4.180

11.0

38.000

100.0

Water
Pigment suspension

Iron Oxide Red

Water

Preparation of the spray

suspension

Polymer solution:
Stir the Kollicoat IR into the specified quantity of water until it has dissolved.
Pigment suspension:
Vigorously stir talc, Iron Oxide Red and titanium dioxide into the specified quantity
of water and homogenize in a high-shear mixer.
Spray suspension:
Stir the pigment suspension into the polymer solution. To avoid sedimentation
during the spraying process, the mixture must be continuously stirred.

03_030724e-11 February 2013

Additional gloss coating

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Kollicoat IR

If a certain appearance of the tablet is needed 5 wt% polyethylene glycol 6000

and Kollidon 17 (at a ratio of 9:1) should be dissolved in water and sprayed after
the spray suspension.
The achieved weight gain should be between 0.30.6 mg/cm2.
Machine parameters
Coating machine

Driacoater type 900, perforated drum coater

Batch size

250 kg

Inlet air temperature

70 C

Outlet air temperature

48 C

Product temperature

50 C

Air flow

4400 m3/h

Atomizing pressure

6 bar

Number of spray nozzles

Spraying rate

700 g/min

Spraying time

55 min

Final drying

60 C/5 min

Quantity applied

3.8%

Tablet properties
Core

Film-coated tablet

Appearance

White

Red

Hardness

93 N

109 N

Friability

0%

0%

Disintegration time

5:53 [min:s]

5:47 [min:s]

Drug release

10 min: 49%
20 min: 98%

10 min: 54%
20 min: 99%

4.2 Instant release coating Caffeine tablets

Composition of the tablets

50 mg caffeine; 229 mg Ludipress; 10 mg Kollidon CL;

40 mg MCC PH 101; 1 mg magnesium stearate

Composition of the spray solution

The formulation is designed for 5 kg of tablets (weight 330 mg; diameter 9 mm)
Proportion [%]
Polymer solution
Kollicoat IR

100.0

19.2

Water

264.0

50.8

Talc

37.4

7.2

Titanium dioxide

18.6

3.6

Water

10.0

19.2

430.0

100

Pigment suspension

03_030724e-11 February 2013

Preparation of the spray

suspension

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Kollicoat IR

Polymer solution:
Stir the Kollicoat IR into the specified quantity of water until it has dissolved.
Pigment suspension:
Vigorously stir talc and titanium dioxide into the specified quantity of water and
homogenize in a high-shear mixer.
Spray suspension:
Stir the pigment suspension into the polymer solution. To avoid sedimentation
during the spraying process, the mixture must be continuously stirred.

Additional gloss coating

If a certain appearance of the tablet is needed 5 wt% polyethylene glycol 6000 and
Kollidon 17 (at a ratio of 9:1) should be dissolved in water and sprayed after the
spray suspension. The achieved weight gain should be between 0.30.6 mg/cm2.
Machine parameters
Coater

Accela-Cota 24, perforated drum coater

Batch size

5 kg

Inlet air temperature

60 C

Outlet air temperature

39 C

Product temperature

35 C

Air flow

180 m3/h

Atomizing pressure

3 bar

Number of spray nozzles

Spraying rate

30 g/min

Spraying time

18 min

Final drying

60 C/4 min

Quantity applied

3 mg/cm2 polymer

Tablet properties
Core

Film-coated tablet

Appearance

White

White

Hardness

116 N

119 N

Friability

0%

0%

Disintegration time

0:58 [min:s]

0:51 [min:s]

Drug release

10 min: 93%
20 min: 92%

10 min: 92%
20 min: 98%

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Kollicoat IR

4.3 Wet binding Acetaminophen instant granules

Composition of the powder mixture

49% acetaminophen, fine powder; 49% sorbitol; 2% aspartame; 0.06% aroma

Composition of the binder solution

The formulation is designed for 1 kg of powder mixture

Weight [g]

Proportion [%]

27.0

15.0

153.0

85.0

180.0

100.0

Granulation solution
Kollicoat IR
Water

Preparation of the binder solution

Stir the Kollicoat IR into the specified quantity of water until it has dissolved.

Manufacture of the granules

Mix the components of the powder mixture for 10 min

(Stephan mixer Type UMC 5 Electronic).
Apply the Kollicoat IR solution in a fine spray, keeping the mixture in motion.
Force the moist mass first through a 3 mm sieve, then a 1 mm sieve.
Dry the moist granules and force them through a 1 mm sieve.

Properties of the granules

The granules dissolve in water within 1 min.

4.4 Drug layering Layering of Riboflavin onto pellets

The pellets consists of sucrose & microcrystalline cellulose.

Pellets size were 2025 mesh.

Coating formulation for the

tracer excipient

Due to surface effects of Riboflavin, the tracer formulation had to be applied with
a solid matter concentration of only 15%.
Weight [g]

Proportion [%]

Granulation solution
Riboflavin

10.0

Kollicoat IR

5.0

Water

85.0

100.0

Coating formulation for the

functional coat (taste masking)

Weight [g]

Proportion [%]

Polymer solution
Kollicoat Smartseal30D

50.5

ATBC
(Acetyltributyl citrate)

7.6
(15% based on pol.)

BHT
(Butylated hydroxytoluene)

1.3
(2.5% based on pol.)

DS
(docusate sodium)

1.0
(2.0% based on pol.)

Talc

39.0

FD & C Blue No. 1

(Brilliant Blue)

1.0
100.0

03_030724e-11 February 2013

Equipments & process details

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Kollicoat IR

Two different coating technologies were used

1. Side vented pan coater (SCP) Perfima Lab with slot drum.
2. Fluid bed coater (FBP) Ghibli Lab, with bottom spray configuration.

Batch size

Coating Pan

FBP

25/30 kg/L

2.53.0 kg/L

Drum speed

18 rpm

Inlet air temperature

7580 C

Inlet air quantity

5568 C

600 m /h

140170

Bore diameter nozzle

1.2 mm

Spray rate

1.2 mm

5070 ml/min

Atomising pressure

25 ml/min

1 bar

1.6 bar

High drug load could be achieved due to high film elasticity of Kollicoat IR.

4.5 Pore former in sustained release coating Propranolol single unit drug delivery system
Composition of the tablet

Weight [g]
Propanolol HCl
(granulated)

163.2

46.62

Ludipress

136.8

39.08

Kollidon VA 64

25.0

7.14

Kollidon CL

20.0

5.71

3.0

0.85

Aerosil 200
Magnesium stearate

Coating parameters

Result

Proportion [%]

2.0

0.57

Total

350.0

100.0

Parameters

Values

Pan

24 Accela-Cota

Batch size

5 kg

Inlet air temperature

60 C

Outlet air volume

216 m3/h

Spray rate

30 gm/min

Drying time

5 mins.

Dissolution profile
Propranolol drug delivery systems dissolution graph
Dissolution [%]
Kollicoat SR 30 D (KSR)
+ Kollicoat IR (KIR)
= drug delivery system

100

CORE
KSR/KIR 5:5
KSR/KIR 6:4
KSR/KIR 7:3
KSR/KIR 8:2

80
60
40
20
0
0

12

16

20

24
time [h]

Kollicoat IR acts as a very effective pore former in conjunction with a functional

polymer to control the drug release.

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Kollicoat IR

4.6 Wet binding Using GranuLac 200

Composition of the powder mixture 95% GranuLac 200 & 5% binder (Kollidon 25, Kollidon 90 & Kollicoat IR)
Composition

The formulation is designed for 1150 g of powder mixture

Material

Weight [g]

Kollicoat IR/Kollidon 30/

Kollidon 90
GranuLac 200

Proportion [%]

57.5

5.0

1092.5

95.0

1150.0

100.0

The binder conc. in the aqueous solution ranges from 5.28.4%.

Preparation of the binder solution

Stir the Kollicoat IR into the specified quantity of water until it has dissolved.

Parameter settings

To get started with Kollicoat IR as a binder

Parameters

Fluid bed granulation

Binder content
in the final granules

3.05.0%

Binder content
in the polymer solution

8.012.0%

Process time

30 minutes

5% is to be preferred for obtaining both strong

granules containing only small amount of fines and
tablets of very high hardness

About 10% is to be preferred to achieve proper

process times & spray rates

By applying the binder solution within 30 minutes

strong granules can be obtained, offering a very
homogeneous particle size distribution.
Spray rate

Standard settings as for PVP

Generally, the higher the spray rate the less fines.

Temperature

Standard settings as for PVP

Generally, the higher the spray rate the less fines.

03_030724e-11 February 2013

Equipment & Process

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Kollicoat IR

Granulator

Fluid bed, Glatt GPCG 3

Set up

Top spray

Nozzle

1.0 mm

Sieve

Oscillating, Erwekaar 400

Batch volume

5L

Batch mass

1150 g

Inlet air temperature

60 C

Air quantity

80110 m3/h

Spray rate

Various

Spray pressure

1.5 bar

Product temperature

Approx. 32 C

Process time

30 minutes

Sieve

800 m

Properties of the granules Kollicoat IR led to much more homogeneous particle size distribution.

Particle size disstribution [-]

1.0
0.8
0.6
0.4
0.2
0.0

16

21
PVP K25

26

16

21

26

PVP K90

16

21

26

Kollicoat IR

Binder/spray rate [g/min]

<125 m

125 355 m

> 355 m

Kollicoat IR led to the formation of strongest granules due to the reason that it
offers elasticity as well as plastic deformation.
Result

The peroxide free Kollicoat IR is an efficient binder combining low viscosity of the
polymer solution and strength of the final agglomerates which in turn led to high
tablets hardness.

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Kollicoat IR

5. Storage conditions

No specific temperature (ambient/room temperature).

6.Stability

At least 2 years in the original sealed containers at room temperature.

7.Toxicology

A toxicological summary is available on request.

8.PRD-No.

30132288

9.Packaging

20 kg plastic drum

Note

This document, or any answers or information provided herein by BASF, doesnot

constitute a legally binding obligation of BASF. While the descriptions, designs,data
and information contained herein are presented in good faith and believed to be
accurate, it is provided for your guidance only. Because many factors may affect
processing or application/use, we recommend that you make tests to determine
the suitability of a product for your particular purpose prior to use. It does not relieve
our customers from the obligation to perform a full inspection of the products upon
delivery or any other obligation. NO WARRANTIES OF ANY KIND, EITHER EXPRESS
OR IMPLIED, INCLUDING WARRANTIES OF MERCHANTABILITY OR FITNESS
FOR A PARTICULAR PURPOSE, ARE MADE REGARDING PRODUCTS DESCRIBED
OR DESIGNS, DATA OR INFORMATION SET FORTH, OR THAT THE PRODUCTS,
DESIGNS, DATA OR INFORMATION MAY BE USED WITHOUT INFRINGING THE
INTELLECTUAL PROPERTY RIGHTS OF OTHERS. IN NO CASE SHALL THE
DESCRIPTIONS, INFORMATION, DATA OR DESIGNS PROVIDED BE CONSIDERED
A PART OF OUR TERMS AND CONDITIONS OF SALE.
February 2013

BASF Nutrition & Health www.pharma-ingredients.basf.com