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Propyl parahydroxybenzoate EUROPEAN PHARMACOPOEIA 5.

Loss on drying (2.2.32). Not more than 0.5 per cent, sodium carbonate solution R ; the substance partly
determined on 1.000 g by drying in an oven at 100-105 °C. dissolves (solution B). Add at the same time to solution A
Sulphated ash (2.4.14). Not more than 0.1 per cent, and solution B 5 ml of aminopyrazolone solution R
determined on 1.0 g. and 1 ml of potassium ferricyanide solution R and mix.
Solution B is yellow to orange-brown. Solution A is
ASSAY orange to red, the colour being clearly more intense than
Dissolve 0.100 g in methanol R and dilute to 250.0 ml with any similar colour which may be obtained with solution B.
the same solvent. Dilute 5.0 ml of the solution to 200.0 ml TESTS
with methanol R. Measure the absorbance (2.2.25) at the
absorption maximum at 275 nm. Solution S. Dissolve 1.0 g in alcohol R and dilute to 10 ml
with the same solvent.
Calculate the content of C10H12O5 taking the specific
absorbance to be 503. Appearance of solution. Solution S is clear (2.2.1) and not
more intensely coloured than reference solution BY6 (2.2.2,
STORAGE Method II).
Protected from light. Acidity. To 2 ml of solution S add 3 ml of alcohol R, 5 ml
IMPURITIES of carbon dioxide-free water R and 0.1 ml of bromocresol
green solution R. Not more than 0.1 ml of 0.1 M sodium
Specified impurities : A. hydroxide is required to change the colour of the indicator
to blue.
Related substances. Thin-layer chromatography (2.2.27).
Test solution (a). Dissolve 0.10 g of the substance to be
examined in acetone R and dilute to 10 ml with the same
solvent.
A. 3,4,5-trihydroxybenzoic acid (gallic acid). Test solution (b). Dilute 1 ml of test solution (a) to 10 ml
with acetone R.
Reference solution (a). Dilute 0.5 ml of test solution (a) to
01/2005:0431 100 ml with acetone R.
Reference solution (b). Dissolve 10 mg of propyl
PROPYL PARAHYDROXYBENZOATE with parahydroxybenzoate CRS in acetone R and dilute to 10 ml
the same solvent.
Propylis parahydroxybenzoas Reference solution (c). Dissolve 10 mg of ethyl
parahydroxybenzoate CRS in 1 ml of test solution (a) and
dilute to 10 ml with acetone R.
Plate : suitable octadecylsilyl silica gel with a fluorescent
indicator having an optimal intensity at 254 nm as the
coating substance.
Mobile phase : glacial acetic acid R, water R, methanol R
(1:30:70 V/V/V).
C10H12O3 Mr 180.2
Application : 2 µl.
DEFINITION Development : over a path of 15 cm.
Propyl 4-hydroxybenzoate. Drying : in air.
Content : 98.0 per cent to 102.0 per cent. Detection : examine in ultraviolet light at 254 nm.
CHARACTERS System suitability : the chromatogram obtained with
Appearance : white, crystalline powder. reference solution (c) shows 2 clearly separated principal
spots.
Solubility : very slightly soluble in water, freely soluble in
alcohol and in methanol. Limits :
— any impurity : any spot in the chromatogram obtained
IDENTIFICATION with test solution (a), apart from the principal spot, is not
First identification : A, B. more intense than the spot in the chromatogram obtained
Second identification : A, C, D. with reference solution (a) (0.5 per cent).
A. Melting point (2.2.14) : 96 °C to 99 °C. Sulphated ash (2.4.14) : maximum 0.1 per cent, determined
B. Infrared absorption spectrophotometry (2.2.24). on 1.0 g.
Comparison : propyl parahydroxybenzoate CRS. ASSAY
C. Examine the chromatograms obtained in the test for To 1.000 g add 20.0 ml of 1 M sodium hydroxide. Heat at
related substances. about 70 °C for 1 h. Cool rapidly in an ice bath. Prepare a
Results : the principal spot in the chromatogram obtained blank in the same manner. Carry out the titration on the
with test solution (b) is similar in position and size to solutions at room temperature. Titrate the excess sodium
the principal spot in the chromatogram obtained with hydroxide with 0.5 M sulphuric acid, continuing the titration
reference solution (b). until the second point of inflexion and determining the
D. To about 10 mg in a test-tube add 1 ml of sodium end-point potentiometrically (2.2.20).
carbonate solution R, boil for 30 s and cool (solution A). 1 ml of 1 M sodium hydroxide is equivalent to 180.2 mg of
To a further 10 mg in a similar test-tube add 1 ml of C10H12O3.

2326 See the information section on general monographs (cover pages)


EUROPEAN PHARMACOPOEIA 5.0 Propylene glycol dicaprylocaprate

IMPURITIES Reducing substances. To 1 ml add 1 ml of dilute


ammonia R1 and heat in a water-bath at 60 °C for 5 min.
The solution is not yellow. Immediately add 0.15 ml of
0.1 M silver nitrate and allow to stand for 5 min. The
solution does not change its appearance.
Heavy metals (2.4.8). Mix 4 ml with 16 ml of water R. 12 ml
of the solution complies with limit test A for heavy metals
A. R = H : 4-hydroxybenzoic acid, (5 ppm m/V). Prepare the reference solution using lead
standard solution (1 ppm Pb) R.
B. R = CH3 : methyl 4-hydroxybenzoate,
Water (2.5.12). Not more than 0.2 per cent, determined on
C. R = CH2-CH3 : ethyl 4-hydroxybenzoate, 5.00 g by the semi-micro determination of water.
D. R = CH2-CH2-CH2-CH3 : butyl 4-hydroxybenzoate. Sulphated ash (2.4.14). Heat 50 g until it burns and ignite.
Allow to cool. Moisten the residue with sulphuric acid R
and ignite ; repeat the operations. The residue weighs not
more than 5 mg (0.01 per cent).
01/2005:0430
STORAGE
PROPYLENE GLYCOL Store in an airtight container.

Propylenglycolum
01/2005:2122

PROPYLENE GLYCOL
DICAPRYLOCAPRATE
C 3 H 8 O2 Mr 76.1
DEFINITION Propylenglycoli dicaprylocapras
Propylene glycol is (RS)-propane-1,2-diol.
DEFINITION
CHARACTERS Propylene glycol diesters of saturated fatty acids, mainly
A viscous, clear, colourless, hygroscopic liquid, miscible with caprylic acid (octanoic acid ; C8H16O2) and capric acid
water and with ethanol (96 per cent). (decanoic acid ; C10H20O2), of vegetable origin.
IDENTIFICATION CHARACTERS
A. It complies with the test for relative density (see Tests). Appearance : almost colourless to light yellow, oily liquid.
B. It complies with the test for refractive index (see Tests). Solubility : practically insoluble in water, soluble in fatty oils
C. Boiling point (2.2.12) : 184 °C to 189 °C. and in light petroleum, slightly soluble in anhydrous ethanol.
D. To 0.5 ml add 5 ml of pyridine R and 2 g of finely ground IDENTIFICATION
nitrobenzoyl chloride R. Boil for 1 min and pour into
15 ml of cold water R with shaking. Filter, wash the A. Refractive index (2.2.6) : 1.439 to 1.442.
precipitate with 20 ml of a saturated solution of sodium B. Relative density (2.2.5) : 0.910 to 0.930.
hydrogen carbonate R and then with water R and dry. C. Viscosity (2.2.9) : 9 mPa·s to 12 mPa·s.
Dissolve in boiling ethanol (80 per cent V/V) R and filter
the hot solution. On cooling, crystals are formed which, D. It complies with the test for composition of fatty acids
after drying at 100-105 °C, melt (2.2.14) at 121 °C to (see Tests).
128 °C.
TESTS
TESTS Appearance. The substance to be examined is clear (2.2.1)
Appearance. It is clear (2.2.1) and colourless (2.2.2, and not more intensely coloured than reference solution BY6
Method II). (2.2.2, Method II).
Relative density (2.2.5) : 1.035 to 1.040. Acid value (2.5.1) : maximum 0.2.
Refractive index (2.2.6) : 1.431 to 1.433. Hydroxyl value (2.5.3, Method A) : maximum 10.
Acidity. To 10 ml add 40 ml of water R and 0.1 ml Iodine value (2.5.4) : maximum 1.0.
of bromothymol blue solution R1. The solution is Peroxide value (2.5.5, Method A) : maximum 1.0.
greenish-yellow. Not more than 0.05 ml of 0.1 M sodium
hydroxide is required to change the colour of the indicator Saponification value (2.5.6) : 320 to 340.
to blue. Unsaponifiable matter (2.5.7) : maximum 0.3 per cent,
Oxidising substances. To 10 ml add 5 ml of water R, 2 ml determined on 5.0 g.
of potassium iodide solution R and 2 ml of dilute sulphuric Alkaline impurities. Dissolve 2.00 g of the substance to be
acid R and allow to stand in a ground-glass-stoppered flask examined in a mixture of 1.5 ml of ethanol (96 per cent) R
protected from light for 15 min. Titrate with 0.05 M sodium and 3.0 ml of ether R. Add 0.05 ml of bromophenol blue
thiosulphate, using 1 ml of starch solution R as indicator. solution R. Not more than 0.15 ml of 0.01 M hydrochloric
Not more than 0.2 ml of 0.05 M sodium thiosulphate is acid is required to change the colour of the indicator to
required. yellow.

General Notices (1) apply to all monographs and other texts 2327

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