Dimeticone

EUROPEAN PHARMACOPOEIA 8.0

IDENTIFICATION
First identification : C.
Second identification : A, B, D.
A. Relative density (2.2.5) : 0.941 to 0.944.
B. Refractive index (2.2.6): 1.435 to 1.439.
C. Infrared absorption spectrophotometry (2.2.24).
Preparation : lms.
Comparison : Ph. Eur. reference spectrum of
dimethylacetamide.
D. Dilute 50 mg with 1 mL of methanol R. Add 1 mL of a 15 g/L
solution of hydroxylamine hydrochloride R and mix. Add
1 mL of dilute sodium hydroxide solution R, mix and allow
to stand for 30 min. Add 1 mL of dilute hydrochloric acid R
and add 1 mL of a 100 g/L solution of ferric chloride R in
0.1 M hydrochloric acid. A reddish-brown colour develops,
reaching a maximum intensity after about 5 min.

total : maximum 0.3 per cent,

disregard limit : the area of the peak in the chromatogram
obtained with reference solution (b) (0.05 per cent).
Heavy metals (2.4.8): maximum 10 ppm.
Dilute 4.0 g to 20.0 mL with water R. 12 mL of the solution
complies with limit test A. Prepare the reference solution
using lead standard solution (2 ppm Pb) R.
Non-volatile matter : maximum 20 ppm.
Evaporate 50 g to dryness using a rotary evaporator at a
pressure not exceeding 1 kPa and on a water-bath. Dry the
residue in an oven at 170-175 C. The residue weighs not
more than 1 mg.
Water (2.5.32) : maximum 0.1 per cent, determined on 0.100 g.

TESTS
Appearance. The substance to be examined is clear (2.2.1)
and not more intensely coloured than reference solution Y7
(2.2.2, Method II).
Acidity. Dilute 50 mL with 50 mL of water R previously
adjusted with 0.02 M potassium hydroxide or 0.02 M
hydrochloric acid to a bluish-green colour, using 0.5 mL of
bromothymol blue solution R1 as indicator. Not more than
5.0 mL of 0.02 M potassium hydroxide is required to restore
the initial (bluish-green) colour.
Alkalinity. To 50 mL add 50 mL of water R previously adjusted
with 0.02 M potassium hydroxide or 0.02 M hydrochloric
acid to a yellow colour, using 0.5 mL of bromothymol blue
solution R1 as indicator. Not more than 0.5 mL of 0.02 M
hydrochloric acid is required to restore the initial (yellow)
colour.
Related substances. Gas chromatography (2.2.28): use the
normalisation procedure.
Test solution. The substance to be examined.
Reference solution (a). Dilute a mixture of 1 mL of the
substance to be examined and 1 mL of dimethylformamide R
to 20 mL with methylene chloride R.
Reference solution (b). Dilute 1 mL of the substance to be
examined to 20.0 mL with methylene chloride R. Dilute 0.1 mL
of the solution to 10.0 mL with methylene chloride R.
Column :
material : fused silica,
size : l = 30 m, = 0.32 mm,
stationary phase : macrogol 20 000 R (lm thickness 1 m).
Carrier gas : nitrogen for chromatography R.
Linear velocity : 30 cm/s.
Split ratio : 1:20.
Temperature :

IMPURITIES

Column

Time
(min)
0 - 15

Temperature
(C)
80 200

Injection port

250

Detector

250

Detection : ame ionisation.

Injection : 0.5 L.
System suitability :
resolution : minimum 5.0 between the peaks due to
dimethylacetamide and impurity B in the chromatogram
obtained with reference solution (a),
signal-to-noise ratio : minimum 10 for the principal peak in
the chromatogram obtained with reference solution (b).
Limits :
any impurity : maximum 0.1 per cent,
General Notices (1) apply to all monographs and other texts

STORAGE
In an airtight container, protected from light.

A. acetic acid,

B. R = H : N,N-dimethylformamide,
C. R = C2H5 : N,N-dimethylpropanamide,
D. R = CH2-CH2-CH3 : N,N-dimethylbutanamide.
07/2013:0138

DIMETICONE
Dimeticonum

[9006-65-9]
DEFINITION
-Trimethylsilyl--methylpoly[oxy(dimethylsilanediyl)].
This poly(dimethylsiloxane) is obtained by hydrolysis
and polycondensation of dichlorodimethylsilane and
chlorotrimethylsilane. Different grades of dimeticone exist
which are distinguished by a number indicating the nominal
kinematic viscosity placed after the name.
Their degree of polymerisation (n = 20 to 400) is such that
their kinematic viscosities are nominally between 20 mm2s 1
and 1300 mm2s 1.
Dimeticones with a nominal viscosity of 50 mm2s 1 or lower
are intended for external use only.
CHARACTERS
Appearance : clear, colourless liquid of various viscosities.
Solubility : practically insoluble in water, very slightly soluble
or practically insoluble in anhydrous ethanol, miscible with
ethyl acetate, with methyl ethyl ketone and with toluene.
IDENTIFICATION
A. It is identied by its kinematic viscosity at 25 C (see Tests).
B. Infrared absorption spectrophotometry (2.2.24).
Comparison : dimeticone CRS.
The region of the spectrum from 850 cm 1 to 750 cm 1 is
not taken into account.

2067

Dimetindene maleate

C. Heat 0.5 g in a test-tube over a small ame until white

fumes begin to appear. Invert the tube over a 2nd tube
containing 1 mL of a 1 g/L solution of chromotropic acid,
sodium salt R in sulfuric acid R so that the fumes reach the
solution. Shake the 2nd tube for about 10 s and heat on a
water-bath for 5 min. The solution is violet.
D. In a platinum crucible, prepare the sulfated ash (2.4.14)
using 50 mg. The residue is a white powder that gives the
reaction of silicates (2.3.1).
TESTS
Acidity. To 2.0 g add 25 mL of a mixture of equal volumes
of anhydrous ethanol R and ether R, previously neutralised
to 0.2 mL of bromothymol blue solution R1, and shake. Not
more than 0.15 mL of 0.01 M sodium hydroxide is required to
change the colour of the solution to blue.
Viscosity (2.2.9): 90 per cent to 110 per cent of the nominal
kinematic viscosity stated on the label, determined at 25 C.
Mineral oils. Place 2 g in a test-tube and examine in ultraviolet
light at 365 nm. The uorescence is not more intense than
that of a solution containing 0.1 ppm of quinine sulfate R in
0.005 M sulfuric acid examined in the same conditions.
Phenylated compounds. Dissolve 5.0 g with shaking in 10 mL
of cyclohexane R. At wavelengths from 250 nm to 270 nm, the
absorbance (2.2.25) of the solution is not greater than 0.2.
Heavy metals : maximum 5 ppm.
Mix 1.0 g with methylene chloride R and dilute to 20 mL
with the same solvent. Add 0.75 mL of a freshly prepared
0.02 g/L solution of dithizone R in methylene chloride R,
0.5 mL of water R and 0.5 mL of a mixture of 1 volume of
dilute ammonia R2 and 9 volumes of a 2 g/L solution of
hydroxylamine hydrochloride R. At the same time, prepare a
reference solution as follows : to 20 mL of methylene chloride R
add 0.75 mL of a freshly prepared 0.02 g/L solution of
dithizone R in methylene chloride R, 0.5 mL of lead standard
solution (10 ppm Pb) R and 0.5 mL of a mixture of 1 volume
of dilute ammonia R2 and 9 volumes of a 2 g/L solution of
hydroxylamine hydrochloride R. Immediately shake each
solution vigorously for 1 min. Any pink colour in the test
solution is not more intense than that in the reference solution.
Volatile matter : maximum 0.3 per cent, for dimeticones with
a nominal viscosity greater than 50 mm2s 1, determined on
1.00 g by heating in an oven at 150 C for 2 h. Carry out the
test using a dish 60 mm in diameter and 10 mm deep.

EUROPEAN PHARMACOPOEIA 8.0

The following characteristic may be relevant for dimeticone

used as emollient.
Viscosity (see Tests).

01/2008:1417
corrected 6.0

DIMETINDENE MALEATE
Dimetindeni maleas

C24H28N2O4
[3614-69-5]

Mr 408.5

DEFINITION
N,N-Dimethyl-2-[3-[(RS)-1-(pyridin-2-yl)ethyl]-1H-inden-2yl]ethanamine (Z)-butenedioate.
Content : 99.0 per cent to 101.0 per cent (dried substance).
CHARACTERS
Appearance : white or almost white, crystalline powder.
Solubility : slightly soluble in water, soluble in methanol.
IDENTIFICATION
Infrared absorption spectrophotometry (2.2.24).
Preparation : discs.
Comparison : dimetindene maleate CRS.

TESTS
Solution S. Dissolve 0.20 g in methanol R and dilute to
20.0 mL with the same solvent.
Appearance of solution. Solution S is clear (2.2.1) and not
more intensely coloured than Y6 (2.2.2, Method II).
LABELLING
Optical
rotation (2.2.7): 0.10 to + 0.10, determined on
The label states :
solution S.
the nominal kinematic viscosity by a number placed after
Related substances. Gas chromatography (2.2.28).
the name of the product ;
where applicable, that the product is intended for external Solvent mixture : acetone R, methylene chloride R (50:50 V/V).
use.
Test solution. Dissolve 50.0 mg of the substance to be
examined in the solvent mixture and dilute to 5.0 mL with the
FUNCTIONALITY-RELATED CHARACTERISTICS
solvent mixture.
This section provides information on characteristics that are
Reference solution (a). Dilute 1 mL of the test solution to
recognised as being relevant control parameters for one or
100.0 mL with the solvent mixture.
more functions of the substance when used as an excipient
Reference solution (b). Dissolve 5.0 mg of 2-ethylpyridine R
(see chapter 5.15). Some of the characteristics described in
(impurity A) in the solvent mixture and dilute to 50.0 mL
the Functionality-related characteristics section may also be
with the solvent mixture. Dilute 10.0 mL of this solution to
present in the mandatory part of the monograph since they
100.0 mL with the solvent mixture.
also represent mandatory quality criteria. In such cases, a
cross-reference to the tests described in the mandatory part is
Column :
included in the Functionality-related characteristics section.
material : fused silica ;
Control of the characteristics can contribute to the quality
size : l = 30 m, = 0.32 mm ;
of a medicinal product by improving the consistency of the
manufacturing process and the performance of the medicinal
stationary phase : polymethylphenylsiloxane R (lm
product during use. Where control methods are cited, they are
thickness 0.25 m).
recognised as being suitable for the purpose, but other methods
can also be used. Wherever results for a particular characteristic Carrier gas : helium for chromatography R.
Linear velocity : about 30 cm/s.
are reported, the control method must be indicated.

2068

See the information section on general monographs (cover pages)