Xylose EUROPEAN PHARMACOPOEIA 11.

Flow rate : 1.0 mL/min.

Detection : spectrophotometer at 220 nm.
Injection : 10 μL.
Relative retention with reference to xylometazoline (retention
time = about 7.2 min): impurity A = about 0.79.
C. [4-(1,1-dimethylethyl)-2,6-dimethylphenyl]acetonitrile,
System suitability : reference solution (b) :
– resolution : minimum 2.5 between the peaks due to
impurity A and xylometazoline.
Limits :
– impurity A : not more than the area of the corresponding
peak in the chromatogram obtained with reference
solution (c) (0.2 per cent) ; D. 1-(1,1-dimethylethyl)-3,5-dimethylbenzene,
– unspecified impurities : for each impurity, not more than the
area of the principal peak in the chromatogram obtained
with reference solution (a) (0.10 per cent) ;
– total : not more than 5 times the area of the principal peak
in the chromatogram obtained with reference solution (a) E. ethane-1,2-diamine mono(4-methylbenzenesulfonate),
(0.5 per cent) ;
– disregard limit : 0.5 times the area of the principal peak in
the chromatogram obtained with reference solution (a)
(0.05 per cent).
Loss on drying (2.2.32) : maximum 0.5 per cent, determined
on 1.000 g by drying in an oven at 105 °C.
F. [4-(1,1-dimethylethyl)-2,6-dimethylphenyl]acetic acid.
Sulfated ash (2.4.14) : maximum 0.1 per cent, determined on
1.0 g.
01/2017:1278
ASSAY
Dissolve 0.200 g in 25 mL of anhydrous acetic acid R and add
10 mL of acetic anhydride R. Titrate with 0.1 M perchloric
acid, determining the end-point potentiometrically (2.2.20).
1 mL of 0.1 M perchloric acid is equivalent to 28.08 mg XYLOSE
of C16H25ClN2.
Xylosum
STORAGE
Protected from light.

IMPURITIES
Specified impurities : A.
Other detectable impurities (the following substances would, C5H10O5 Mr 150.1
if present at a sufficient level, be detected by one or other of [58-86-6]
the tests in the monograph. They are limited by the general
acceptance criterion for other/unspecified impurities and/or DEFINITION
by the general monograph Substances for pharmaceutical use D-Xylopyranose.
(2034). It is therefore not necessary to identify these impurities
for demonstration of compliance. See also 5.10. Control of CHARACTERS
impurities in substances for pharmaceutical use) : B, C, D, E, F. Appearance : white or almost white, crystalline powder or
colourless needles.
Solubility : freely soluble in water, soluble in hot ethanol
(96 per cent).
IDENTIFICATION
First identification : A.
Second identification : B, C.
A. N-(2-aminoethyl)-2-[4-(1,1-dimethylethyl)-2,6- A. Infrared absorption spectrophotometry (2.2.24).
dimethylphenyl]acetamide, Preparation : discs.
Comparison : xylose CRS.
B. Thin-layer chromatography (2.2.27).
Solvent mixture : water R, methanol R (2:3 V/V).
Test solution. Dissolve 10 mg of the substance to be
examined in the solvent mixture and dilute to 20 mL with
the solvent mixture.
Reference solution (a). Dissolve 10 mg of xylose CRS in
B. 2-(chloromethyl)-5-(1,1-dimethylethyl)-1,3- the solvent mixture and dilute to 20 mL with the solvent
dimethylbenzene, mixture.

4410 See the information section on general monographs (cover pages)

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EUROPEAN PHARMACOPOEIA 11.0
Reference solution (b). Dissolve 10 mg of fructose R, 10 mg
of glucose R and 10 mg of xylose R in the solvent mixture
and dilute to 20 mL with the solvent mixture.
Plate : TLC silica gel plate R.
Mobile phase : water R, methanol R, anhydrous acetic acid R,
ethylene chloride R (10:15:25:50 V/V/V/V) ; measure the
volumes accurately since a slight excess of water produces
cloudiness.
Application : 2 μL ; thoroughly dry the points of application.
Development : over a path of 15 cm.
Drying : in a current of warm air.
Detection : spray with a 5 g/L solution of thymol R in a
mixture of 5 volumes of sulfuric acid R and 95 volumes
of ethanol (96 per cent) R. Heat in an oven at 130 °C for
10 min.
System suitability : reference solution (b):
– the chromatogram shows 3 clearly separated spots.
Results : the principal spot in the chromatogram obtained
with the test solution is similar in position, colour and size
to the principal spot in the chromatogram obtained with
reference solution (a).
C. Dissolve 0.1 g in 10 mL of water R. Add 3 mL of
cupri-tartaric solution R and heat. An orange or red
precipitate is formed.
General Notices (1) apply to all monographs and other texts
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Xylose
TESTS
Solution S. Dissolve 10.0 g in carbon dioxide-free water R and
dilute to 100 mL with the same solvent.
Appearance of solution. Solution S is clear (2.2.1) and
colourless (2.2.2, Method II).
Acidity or alkalinity. To 50 mL of solution S add 0.3 mL of
phenolphthalein solution R1. The solution is colourless. Not
more than 0.2 mL of 0.1 M sodium hydroxide is required to
change the colour of the indicator to pink.
Specific optical rotation (2.2.7) : + 18.5 to + 19.5 (dried
substance).
Dissolve 10.0 g in 80 mL of water R, add 1 mL of dilute
ammonia R2 and dilute to 100.0 mL with water R. Allow to
stand for 30 min.
Chlorides (2.4.4) : maximum 330 ppm.
Dilute 1.5 mL of solution S to 15 mL with water R.
Loss on drying (2.2.32) : maximum 0.5 per cent, determined
on 1.000 g by drying in an oven at 105 °C at a pressure not
exceeding 0.7 kPa.
Sulfated ash (2.4.14): maximum 0.1 per cent, determined on
1.0 g.
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