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Barbital EUROPEAN PHARMACOPOEIA 5.

chromatogram obtained with reference solution (b) (0.6 per DEFINITION


cent). Disregard any peak due to the mobile phase and Barbital contains not less than 99.0 per cent and
any peak with an area less than 0.25 times the area of the not more than the equivalent of 101.0 per cent of
principal peak obtained with reference solution (b). 5,5-diethylpyrimidine-2,4,6(1H,3H,5H)-trione, calculated
Water (2.5.12). Not more than 0.5 per cent, determined on with reference to the dried substance.
0.500 g by the semi-micro determination of water.
CHARACTERS
Sulphated ash (2.4.14). Not more than 0.1 per cent, A white, crystalline powder or colourless crystals, slightly
determined on 1.0 g. soluble in water, soluble in boiling water and in alcohol. It
ASSAY forms water-soluble compounds with alkali hydroxides and
carbonates and with ammonia.
Dissolve 0.320 g in 50 ml of alcohol R and add 5 ml of 0.01 M
hydrochloric acid. Carry out a potentiometric titration IDENTIFICATION
(2.2.20), using 0.1 M sodium hydroxide. Read the volume First identification : A, B.
added between the two points of inflexion.
Second identification : A, C, D.
1 ml of 0.1 M sodium hydroxide is equivalent to 40.39 mg
of C18H30ClN3O5. A. Determine the melting point (2.2.14) of the substance
to be examined. Mix equal parts of the substance to be
IMPURITIES examined and barbital CRS and determine the melting
point of the mixture. The difference between the melting
points (which are about 190 C) is not greater than 2 C.
B. Examine by infrared absorption spectrophotometry
(2.2.24), comparing with the spectrum obtained with
barbital CRS.
C. Examine by thin-layer chromatography (2.2.27), using
silica gel GF254 R as the coating substance.
Test solution. Dissolve 75 mg of the substance to be
A. R1 = NH-C(CH3)3, R2 = R3 = H : (1RS)-1-(3,5- examined in alcohol R and dilute to 25 ml with the same
dihydroxyphenyl)-2-[(1,1-dimethylethyl)amino]ethanol solvent.
(terbutaline), Reference solution. Dissolve 75 mg of barbital CRS in
B. R1 = OH, R2 = R3 = CO-N(CH3)2 : 5-[(1RS)-1,2- alcohol R and dilute to 25 ml with the same solvent.
dihydroxyethyl]-1,3-phenylene bis(dimethylcarbamate), Apply separately to the plate 10 l of each solution.
Develop over a path of 18 cm using the lower layer of
C. R1 = NH-C(CH3)3, R2 = H, R3 = CO-N(CH3)2 : 3-[(1RS)-2-[(1, a mixture of 5 volumes of concentrated ammonia R,
1-dimethylethyl)amino]-1-hydroxyethyl]-5-hydroxyphenyl 15 volumes of alcohol R and 80 volumes of chloroform R.
dimethylcarbamate, Examine immediately in ultraviolet light at 254 nm. The
D. R1 = H, R2 = R3 = CO-N(CH3)2 : 5-[(1RS)-1-hydroxyethyl]- principal spot in the chromatogram obtained with the test
1,3-phenylene bis(dimethylcarbamate), solution is similar in position and size to the principal
spot in the chromatogram obtained with the reference
solution.
D. It gives the reaction of non-nitrogen substituted
barbiturates (2.3.1).
TESTS
Appearance of solution. Dissolve 1.0 g in a mixture of 4 ml
of dilute sodium hydroxide solution R and 6 ml of water R.
The solution is clear (2.2.1) and not more intensely coloured
than reference solution Y6 (2.2.2, Method II).
E. R = H : 5-acetyl-1,3-phenylene bis(dimethylcarbamate), Acidity. Boil 1.0 g with 50 ml of water R for 2 min, allow to
cool and filter. To 10 ml of the filtrate add 0.15 ml of methyl
F. R = NH-C(CH3)3 : 5-[[(1,1-dimethylethyl)amino]acetyl]-1,
red solution R. The solution is orange-yellow. Not more than
3-phenylene bis(dimethylcarbamate).
0.1 ml of 0.1 M sodium hydroxide is required to produce
a pure yellow colour.
Related substances. Examine by thin-layer chromatography
01/2005:0170 (2.2.27), using silica gel GF254 R as the coating substance.
Test solution. Dissolve 1.0 g of the substance to be examined
BARBITAL in alcohol R and dilute to 100 ml with the same solvent.
Reference solution. Dilute 0.5 ml of the test solution to
Barbitalum 100 ml with alcohol R.
Apply separately to the plate 20 l of each solution. Develop
over a path of 15 cm using the lower layer of a mixture
of 5 volumes of concentrated ammonia R, 15 volumes
of alcohol R and 80 volumes of chloroform R. Examine
immediately in ultraviolet light at 254 nm. Spray with
diphenylcarbazone mercuric reagent R. Allow the plate
to dry in air and spray with freshly prepared alcoholic
C8H12N2O3 Mr 184.2 potassium hydroxide solution R diluted 1 in 5 with

1052 See the information section on general monographs (cover pages)


EUROPEAN PHARMACOPOEIA 5.0 Basic butylated methacrylate copolymer

aldehyde-free alcohol R. Heat at 100 C to 105 C for 5 min and shake well. The colour of the solution is more intense
and examine immediately. When examined in ultraviolet than that of a standard prepared at the same time and in the
light and after spraying, any spot in the chromatogram same manner omitting the potassium iodate.
obtained with the test solution, apart from the principal Soluble barium salts. To 10 ml of solution S add 1 ml of
spot, is not more intense than the spot in the chromatogram dilute sulphuric acid R. After 1 h, any opalescence in the
obtained with the reference solution (0.5 per cent). solution is not more intense than that in a mixture of 10 ml
Loss on drying (2.2.32). Not more than 0.5 per cent, of solution S and 1 ml of distilled water R.
determined on 1.00 g by drying in an oven at 100 C to Phosphates. To 1.0 g add a mixture of 3 ml of dilute nitric
105 C. acid R and 7 ml of water R. Heat on a water-bath for 5 min,
Sulphated ash (2.4.14). Not more than 0.1 per cent, filter and dilute the filtrate to 10 ml with water R. Add
determined on 1.0 g. 5 ml of molybdovanadic reagent R. After 5 min, any yellow
colour in the test solution is not more intense than that in a
ASSAY standard prepared at the same time and in the same manner
Dissolve 85.0 mg in 5 ml of pyridine R. Add 0.5 ml of using 10 ml of phosphate standard solution (5 ppm PO4) R
thymolphthalein solution R and 10 ml of silver nitrate (50 ppm).
solution in pyridine R. Titrate with 0.1 M ethanolic sodium Arsenic (2.4.2). In a small long-necked combustion flask,
hydroxide until a pure blue colour is obtained. Carry out shake 0.5 g with 2 ml of nitric acid R and 30 ml of water R,
a blank titration. insert a small funnel in the neck of the flask, heat in an
1 ml of 0.1 M ethanolic sodium hydroxide is equivalent to inclined position on a water-bath for 2 h, allow to cool, adjust
9.21 mg of C8H12N2O3. to the original volume with water R and filter. Wash the
residue by decantation with three quantities, each of 5 ml,
01/2005:0010 of water R. Combine the filtrate and washings, add 1 ml of
sulphuric acid R, evaporate to dryness on a water-bath, and
BARIUM SULPHATE heat until copious white fumes are evolved. Dissolve the
residue in 10 ml of dilute sulphuric acid R and add 10 ml of
Barii sulfas water R. The solution complies with limit test A for arsenic
(2 ppm).
BaSO4 Mr 233.4 Heavy metals (2.4.8). Dilute 10 ml of solution S to 20 ml
with water R, 12 ml of this solution complies with limit test A
CHARACTERS for heavy metals (10 ppm). Prepare the standard using lead
A fine, heavy, white powder, free from gritty particles, standard solution (1 ppm Pb) R.
practically insoluble in water and in organic solvents. It Loss on ignition. Not more than 2.0 per cent, determined on
is very slightly soluble in acids and in solutions of alkali 1.0 g at 600 C.
hydroxides.
Sedimentation. Place 5.0 g in a glass-stoppered, 50 ml
IDENTIFICATION graduated cylinder having the 50 ml graduation mark 14 cm
A. Boil 0.2 g with 5 ml of a 500 g/l solution of sodium from the base. Add water R to 50 ml, shake the mixture for
carbonate R for 5 min, add 10 ml of water R, filter and 5 min and allow to stand for 15 min. The barium sulphate
acidify a part of the filtrate with dilute hydrochloric does not settle below the 15 ml mark.
acid R. The solution gives the reactions of sulphates
(2.3.1). 01/2005:1975
B. Wash the residue collected in the preceding test with
three successive small quantities of water R. To the BASIC BUTYLATED METHACRYLATE
residue add 5 ml of dilute hydrochloric acid R, filter and COPOLYMER
add to the filtrate 0.3 ml of dilute sulphuric acid R. A
white precipitate is formed that is insoluble in dilute Copolymerum methacrylatis butylati
sodium hydroxide solution R.
basicum
TESTS
DEFINITION
Solution S. To 20.0 g add 40 ml of distilled water R and
60 ml of dilute acetic acid R. Boil for 5 min, filter and dilute Copolymer of 2-(dimethylamino)ethyl methacrylate, butyl
the cooled filtrate to 100 ml with distilled water R. methacrylate and methyl methacrylate having a mean
relative molecular mass of about 150 000. The ratio
Acidity or alkalinity. Heat 5.0 g with 20 ml of carbon of 2-dimethylaminoethyl methacrylate groups to butyl
dioxide-free water R on a water-bath for 5 min and filter. methacrylate and methyl methacrylate groups is about 2:1:1.
To 10 ml of the filtrate add 0.05 ml of bromothymol blue
solution R1. Not more than 0.5 ml of 0.01 M hydrochloric Content of dimethylaminoethyl groups: 20.8 per cent to
acid or 0.01 M sodium hydroxide is required to change the 25.5 per cent (dried substance).
colour of the indicator. CHARACTERS
Acid-soluble substances. Evaporate 25 ml of solution S Appearance : colourless or yellowish granules or white
to dryness on a water-bath and dry to constant mass at powder, slightly hygroscopic.
100-105 C. The residue weighs not more than 15 mg Solubility : practically insoluble in water, freely soluble in
(0.3 per cent). methylene chloride. It dissolves slowly in alcohol.
Oxidisable sulphur compounds. Shake 1.0 g with 5 ml of
water R for 30 s and filter. To the filtrate add 0.1 ml of IDENTIFICATION
starch solution R, dissolve 0.1 g of potassium iodide R in the A. Infrared absorption spectrophotometry (2.2.24).
mixture, add 1.0 ml of a freshly prepared 3.6 mg/l solution Comparison : Ph. Eur. reference spectrum of basic
of potassium iodate R and 1 ml of 1 M hydrochloric acid butylated methacrylate copolymer.

General Notices (1) apply to all monographs and other texts 1053