Calcium stearate

EUROPEAN PHARMACOPOEIA 5.0

Fluorides. Not more than 75 ppm of F, determined

potentiometrically (2.2.36, Method I) using a
fluoride-selective indicator electrode and a silver-silver
chloride reference electrode.
Test solution. In a 50 ml volumetric flask, dissolve 0.250 g
in 0.1 M hydrochloric acid, add 5.0 ml of fluoride standard
solution (1 ppm F) R and dilute to 50.0 ml with 0.1 M
hydrochloric acid. To 20.0 ml of the solution add 20.0 ml
of total-ionic-strength-adjustment buffer R and 3 ml of an
82 g/l solution of anhydrous sodium acetate R. Adjust to
pH 5.2 with ammonia R and dilute to 50.0 ml with distilled
water R.
Reference solutions. To 5.0 ml, 2.0 ml, 1.0 ml, 0.5 ml and
0.25 ml of fluoride standard solution (10 ppm F) R add
20.0 ml of total-ionic-strength-adjustment buffer R and
dilute to 50.0 ml with distilled water R.
Carry out the measurements on 20.0 ml of each solution.
Calculate the concentration of fluorides using the calibration
curve, taking into account the addition of fluoride to the
test solution.
Sulphates (2.4.13). Dilute 1 ml of solution S to 25 ml with
distilled water R. 15 ml of the solution complies with the
limit test for sulphates (0.5 per cent).
ASSAY
Dissolve 0.180 g in 50 ml of anhydrous acetic acid R.
Arsenic (2.4.2). 5 ml of solution S complies with limit test A
Titrate with 0.1 M perchloric acid determining the end-point for arsenic (4 ppm).
potentiometrically (2.2.20).
Iron (2.4.9). Dilute 0.5 ml of solution S to 10 ml with
1 ml of 0.1 M perchloric acid is equivalent to 23.83 mg of
water R. The solution complies with the limit test for iron
C18H32CaN2O10.
(400 ppm).
Heavy metals (2.4.8). Dilute 13 ml of solution S to 20 ml
STORAGE
with water R. 12 ml of the solution complies with limit test A
Store in an airtight container.
for heavy metals (30 ppm). Prepare the standard using lead
standard solution (1 ppm Pb) R.
01/2005:1052 Acid-insoluble matter. Dissolve 5.0 g in a mixture of 10 ml
of hydrochloric acid R and 30 ml of water R. Filter, wash
CALCIUM PHOSPHATE
the residue with water R and dry to constant mass at 100 C
to 105 C. The residue weighs not more than 10 mg (0.2 per
cent).
Tricalcii phosphas
Loss on ignition. Not more than 8.0 per cent, determined on
DEFINITION
1.000 g by ignition at 800 C for 30 min.
Calcium phosphate consists of a mixture of calcium
phosphates. It contains not less than 35.0 per cent and not ASSAY
more than the equivalent of 40.0 per cent of Ca (Ar 40.08).
Dissolve 0.200 g in a mixture of 1 ml of hydrochloric acid R1
and 5 ml of water R. Add 25.0 ml of 0.1 M sodium edetate
CHARACTERS
and dilute to 200 ml with water R. Adjust to about pH 10
A white or almost white powder, practically insoluble in
with concentrated ammonia R. Add 10 ml of ammonium
water. It dissolves in dilute hydrochloric acid and in dilute
chloride buffer solution pH 10.0 R and a few milligrams
nitric acid.
of mordant black 11 triturate R. Titrate the excess sodium
edetate with 0.1 M zinc sulphate until the colour changes
IDENTIFICATION
from blue to violet.
A. Dissolve 0.1 g in 5 ml of a 25 per cent V/V solution
1 ml of 0.1 M sodium edetate is equivalent to 4.008 mg of Ca.
of nitric acid R. The solution gives reaction (b) of
phosphates (2.3.1).
B. It gives reaction (b) of calcium (2.3.1). Filter before
01/2005:0882
adding potassium ferrocyanide solution R.
Reference solution (a). Dissolve 20 mg of calcium
pantothenate CRS in water R and dilute to 5 ml with the
same solvent.
Reference solution (b). Dissolve 10 mg of 3-aminopropionic
acid R in water R and dilute to 50 ml with the same solvent.
Apply separately to the plate 5 l of each solution. Develop
over a path of 12 cm using a mixture of 35 volumes of water R
and 65 volumes of ethanol R. Dry the plate in a current of
air and spray with ninhydrin solution R1. Heat at 110 C
for 10 min. Any spot corresponding to 3-aminopropionic acid
in the chromatogram obtained with test solution (a) is not
more intense than the spot in the chromatogram obtained
with reference solution (b) (0.5 per cent).
Chlorides (2.4.4). 5 ml of solution S diluted to 15 ml with
water R complies with the limit test for chlorides (200 ppm).
Heavy metals (2.4.8). 12 ml of solution S complies with limit
test A for heavy metals (20 ppm). Prepare the standard using
lead standard solution (1 ppm Pb) R.
Loss on drying (2.2.32). Not more than 3.0 per cent,
determined on 1.000 g by drying in an oven at 100 C to
105 C.

C. It complies with the limits of the assay.

CALCIUM STEARATE

TESTS
Solution S. Dissolve 2.50 g in 20 ml of dilute hydrochloric
acid R. If the solution is not clear, filter it. Add dilute
ammonia R1 dropwise until a precipitate is formed. Dissolve
the precipitate by adding dilute hydrochloric acid R and
dilute to 50 ml with distilled water R.
Chlorides (2.4.4). Dissolve 0.22 g in a mixture of 1 ml of
nitric acid R and 10 ml of water R and dilute to 100 ml with
water R. 15 ml of the solution complies with the limit test
for chlorides (0.15 per cent).

DEFINITION
Calcium stearate is a mixture of calcium salts of different
fatty acids consisting mainly of stearic acid [(C17H35COO)2Ca ;
Mr 607] and palmitic acid [(C15H31COO)2Ca ; Mr 550.9] with
minor proportions of other fatty acids. It contains not less
than 6.4 per cent and not more than 7.4 per cent of Ca (Ar
40.08), calculated with reference to the dried substance. The

General Notices (1) apply to all monographs and other texts

1167

Calcii stearas

Calcium stearate

EUROPEAN PHARMACOPOEIA 5.0

Measure the absorbance at 228.8 nm using a cadmium

hollow-cathode lamp as source of radiation and a graphite
furnace as atomic generator.
Lead. Not more than 10 ppm of Pb, determined by atomic
CHARACTERS
absorption spectrometry (2.2.23, Method II).
A fine, white or almost white, crystalline powder, practically Test solution. Use the solution described in the test for
cadmium.
insoluble in water and in alcohol.
Reference solutions. Prepare the reference solutions using
lead standard solution (10 ppm Pb) R, diluted if necessary
IDENTIFICATION
with
water R.
First identification : C, D.
Measure the absorbance at 283.3 nm using a lead
Second identification : A, B, D.
hollow-cathode lamp as source of radiation and a graphite
A. The residue obtained in the preparation of solution S (see furnace as atomic generator. Depending on the apparatus,
Tests) has a freezing point (2.2.18) not lower than 53 C. the line at 217.0 nm may be used.
Nickel. Not more than 5 ppm of Ni, determined by atomic
B. The acid value of the fatty acids (2.5.1) is 195 to 210,
absorption spectrometry (2.2.23, Method II).
determined on 0.200 g of the residue obtained in the
preparation of solution S dissolved in 25 ml of the
Test solution. Use the solution described in the test for
prescribed mixture of solvents.
cadmium.
Reference solutions. Prepare the reference solutions using
C. Examine the chromatograms obtained in the test for
nickel standard solution (10 ppm Ni) R, diluted if necessary
fatty acid composition. The retention times of the
with water R.
principal peaks in the chromatogram obtained with the
test solution are approximately the same as those of the
Measure the absorbance at 232.0 nm using a nickel
principal peaks in the chromatogram obtained with the
hollow-cathode lamp as source of radiation and a graphite
reference solution.
furnace as atomic generator.
D. Neutralise 5 ml of solution S to red litmus paper R using Loss on drying (2.2.32). Not more than 6.0 per cent,
strong sodium hydroxide solution R. The solution gives determined on 1.000 g by drying in an oven at 100-105 C.
reaction (b) of calcium (2.3.1).
Microbial contamination. Total viable aerobic count (2.6.12)
not more than 103 micro-organisms per gram, determined
TESTS
by plate count. It complies with the test for Escherichia
coli (2.6.13).
Solution S. To 5.0 g add 50 ml of peroxide-free ether R,
20 ml of dilute nitric acid R and 20 ml of distilled water R.
Boil under a reflux condenser until dissolution is complete. ASSAY
Allow to cool. In a separating funnel, separate the aqueous Calcium. To 0.500 g in a 250 ml conical flask add 50 ml of a
layer and shake the ether layer with 2 quantities, each of
mixture of equal volumes of butanol R and ethanol R, 5 ml
5 ml, of distilled water R. Combine the aqueous layers, wash of concentrated ammonia R, 3 ml of ammonium chloride
with 15 ml of peroxide-free ether R and dilute the aqueous buffer solution pH 10.0 R, 30.0 ml of 0.1 M sodium edetate
layer to 50 ml with distilled water R (solution S). Evaporate and 15 mg of mordant black 11 triturate R. Heat to 45-50 C
the ether layer to dryness and dry the residue at 100-105 C. until the solution is clear. Cool and titrate with 0.1 M zinc
Keep the residue for identification tests A and B.
sulphate until the colour changes from blue to violet. Carry
out a blank titration.
Acidity or alkalinity. To 1.0 g add 20 ml of carbon
dioxide-free water R and boil for 1 min with continuous
1 ml of 0.1 M sodium edetate is equivalent to 4.008 mg of Ca.
shaking. Cool and filter. To 10 ml of the filtrate add 0.05 ml
Fatty acid composition. Examine by gas chromatography
of bromothymol blue solution R1. Not more than 0.5 ml of
(2.2.28).
0.01 M hydrochloric acid or 0.01 M sodium hydroxide is
Test solution. In a conical flask fitted with a reflux
required to change the colour of the indicator.
condenser, dissolve 0.10 g of the substance to be examined in
Chlorides (2.4.4). Dilute 0.5 ml of solution S to 15 ml
5 ml of boron trifluoride-methanol solution R. Boil under a
with water R. The solution complies with the limit test for
reflux condenser for 10 min. Add 4 ml of heptane R through
chlorides (0.1 per cent).
the condenser and boil again under a reflux condenser for
Sulphates (2.4.13). Dilute 0.5 ml of solution S to 15 ml with 10 min. Allow to cool. Add 20 ml of a saturated sodium
distilled water R. The solution complies with the limit test
chloride solution R. Shake and allow the layers to separate.
for sulphates (0.3 per cent).
Remove about 2 ml of the organic layer and dry over 0.2 g of
anhydrous sodium sulphate R. Dilute 1.0 ml of the solution
Cadmium. Not more than 3 ppm of Cd, determined by
to 10.0 ml with heptane R.
atomic absorption spectrometry (2.2.23, Method II).
Reference solution. Prepare the reference solution in the
Test solution. Place 50.0 mg of the substance to be examined same manner as the test solution using 50.0 mg of palmitic
in a polytetrafluoroethylene digestion bomb and add
acid CRS and 50.0 mg of stearic acid CRS instead of calcium
0.5 ml of a mixture of 1 volume of hydrochloric acid R and stearate.
5 volumes of cadmium- and lead-free nitric acid R. Allow to
digest at 170 C for 5 h. Allow to cool. Dissolve the residue The chromatographic procedure may be carried out using :
in water R and dilute to 5.0 ml with the same solvent.
a fused-silica column 30 m long and 0.32 mm in internal
diameter coated with macrogol 20 000 R (film thickness
Reference solutions. Prepare the reference solutions using
0.5 m),
cadmium standard solution (10 ppm Cd) R, diluted if
necessary with a 1 per cent V/V solution of hydrochloric
helium for chromatography R as the carrier gas at a flow
acid R.
rate of 2.4 ml/min,
fatty acid fraction contains not less than 40.0 per cent of
stearic acid and the sum of stearic acid and palmitic acid is
not less than 90.0 per cent.

1168

See the information section on general monographs (cover pages)

Calendula flower

EUROPEAN PHARMACOPOEIA 5.0

Iron (2.4.9). To 0.25 g add a mixture of 5 ml of hydrochloric

acid R and 20 ml of water R. Heat to boiling, cool and filter.
10 ml of the filtrate complies with the limit test for iron
Time
Temperature
Rate
Comment
(100 ppm).
(min)
(C)
(C/min)
Heavy metals (2.4.8). To 2.5 g add a mixture of 2 ml of
0-2
70
isothermal
Column
hydrochloric acid R and 15 ml of water R. Heat to boiling.
2 - 36
70 240
5
Cool and then add 0.5 ml of phenolphthalein solution R.
linear gradient
Cautiously add concentrated ammonia R until the colour
240
36 - 41
isothermal
changes to pink. Add 0.5 ml of glacial acetic acid R and
Injection port
220
dilute to 25 ml with water R. Filter. 12 ml of the filtrate
complies with limit test A for heavy metals (20 ppm). Prepare
Detector
260
the standard using lead standard solution (2 ppm Pb) R.
Inject 1 l of the reference solution. When the chromatogram Loss on ignition : 18.0 per cent to 22.0 per cent, determined
is recorded in the prescribed conditions, the retention time
on 1.000 g by ignition to constant mass at 800 C.
of methyl palmitate relative to that of methyl stearate is
about 0.88. The test is not valid unless, in the chromatogram ASSAY
obtained with the reference solution, the resolution between Dissolve 0.150 g in 120 ml of water R. Carry out the
the peaks corresponding to methyl stearate and methyl
complexometric titration of calcium (2.5.11).
palmitate is at least 5.0.
1 ml of 0.1 M sodium edetate is equivalent to 17.22 mg of
Inject 1 l of the test solution. Calculate the percentage
CaSO4,2H2O.
content of stearic acid and palmitic acid from the areas of the
peaks in the chromatogram obtained with the test solution
by the normalisation procedure, disregarding the peak due
01/2005:1297
to the solvent.
a flame-ionisation detector,
with the following temperature programme :

CALENDULA FLOWER
01/2005:0982

CALCIUM SULPHATE DIHYDRATE

Calendulae flos

DEFINITION
Calendula flower consists of the whole or cut, dried, and
Calcii sulfas dihydricus
fully opened flowers which have been detached from the
receptacle of the cultivated, double-flowered varieties of
CaSO4,2H2O
Mr 172.2 Calendula officinalis L. It contains not less than 0.4 per cent
of flavonoids, calculated as hyperoside (C21H20O12, Mr 464.4)
DEFINITION
with reference to the dried drug.
Calcium sulphate dihydrate contains not less than 98.0 per
CHARACTERS
cent and not more than the equivalent of 102.0 per cent of
CaSO4,2H2O.
It has the macroscopic and microscopic characters described
under identification tests A and B.
CHARACTERS
IDENTIFICATION
A white, fine powder, very slightly soluble in water,
practically insoluble in alcohol.
A. The ligulate florets consist of a yellow or orange-yellow
ligule, about 3 mm to 5 mm wide and about 7 mm in the
IDENTIFICATION
middle part, with a three toothed apex and a hairy, partly
A. It complies with the test for loss on ignition (see Tests).
sickle-shaped yellowish-brown to orange-brown tube with
a projecting style and a bifid stigma occasionally with a
B. Solution S (see Tests) gives reaction (a) of sulphates
partly bent yellowish-brown to orange-brown ovary. The
(2.3.1).
tubular florets, about 5 mm long, are present and consist
C. Solution S gives reaction (a) of calcium (2.3.1).
of the yellow, orange-red or red-violet five lobed corolla
and the yellowish-brown or orange-brown tube, hairy in
TESTS
its lower part, mostly with a partly bent yellowish-brown
Solution S. Dissolve 1.0 g in 50 ml of a 10 per cent V/V
to orange-brown ovary.
solution of hydrochloric acid R by heating at 50 C for
B. Reduce to a powder (355). The powder is yellowish-brown.
5 min. Allow the solution to cool.
Examine under a microscope using chloral hydrate
Acidity or alkalinity. Shake 1.5 g with 15 ml of carbon
solution R. The powder shows fragments of the corollas
dioxide-free water R for 5 min. Allow to stand for 5 min and
containing light yellow oil droplets, some with fairly
filter. To 10 ml of the filtrate, add 0.1 ml of phenolphthalein
large anomocytic stomata (2.8.3), others containing
solution R and 0.25 ml of 0.01 M sodium hydroxide.
prisms and very small cluster crystals of calcium oxalate ;
The solution is red. Add 0.30 ml of 0.01 M hydrochloric
covering trichomes biseriate, multicellular and conical,
acid. The solution is colourless. Add 0.2 ml of methyl red
glandular trichomes with a uniseriate or biseriate,
solution R. The solution is reddish-orange.
multicellular biseriate stalk and a large, ovoid, biseriate
Chlorides (2.4.4). Shake 0.5 g with 15 ml of water R for
and multicellular head ; spherical pollen grains up to
5 min. Allow to stand for 15 min and filter. Dilute 5 ml of the
about 40 m in diameter with a sharply spiny exine and
filtrate to 15 ml with water R. The solution complies with
three germinal pores ; occasional fragments of the stigmas
the limit test for chlorides (300 ppm).
with short, bulbous papillae.
Arsenic (2.4.2). 5 ml of solution S complies with limit test A C. Examine by thin-layer chromatography (2.2.27), using a
suitable silica gel as the coating substance.
for arsenic (10 ppm).
General Notices (1) apply to all monographs and other texts

1169