欧洲药典-羧甲基纤维素Carmellose
Carmellose EUROPEAN PHARMACOPOEIA
7.0Development :over a path of 15cm.
Drying :in air for 15min.
Detection :spray with a solution prepared as follows:dissolve 5g of phosphomolybdic acid R in a mixture of 50mL of glacial acetic acid R and 10mL of sulfuric acid R ,and dilute to
100mL
with glacial acetic acid R .Heat the plate at 100-105°C for 30min.System suitability :
—the chromatogram obtained with reference solution (c)shows 1clearly visible spot,—the chromatogram obtained with reference solution (e)shows 2clearly separated spots.Limits :in the chromatogram obtained with test solution (a):
—impurity D :any spot due to impurity D is not more intense
than the spot in the chromatogram obtained with reference solution (a)(0.5per cent),—any other impurity
:any spot,apart from the principal
spot and any spot due to impurity D,is not more intense than the spot in the chromatogram obtained with reference solution (b)(0.2per cent).Heavy metals (2.4.8):maximum 10ppm.2.0g complies with limit test C.Prepare the standard using 2mL of lead standard solution (10ppm Pb)R .Loss on drying (2.2.32):maximum 0.5per cent,determined on 1.000g in vacuo at 60°C for 3h.Sulfated ash (2.4.14):maximum 0.1per cent,determined on 1.0g.ASSAY Dissolve 0.100g in 15mL of a 25per cent V/V solution of sulfuric acid R and boil under a reflux condenser for 3h.Cool,dissolve by cautiously adding 30mL of water R ,cool again and place in a steam-distillation apparatus.Add 40mL of strong sodium hydroxide solution R and distil immediately by passing steam through the mixture.Collect the distillate into 40mL of a 40g/L solution of boric acid R until the total volume in the receiver reaches about 200mL.Add 0.25mL of methyl red mixed solution R .Titrate with 0.1M hydrochloric acid ,
until the colour changes from green to violet.Carry out a blank titration.1mL of 0.1M hydrochloric acid is equivalent to 13.02mg of C 12H 24N 2O 4.
IMPURITIES A.(2RS )-2-(hydroxymethyl)-2-methylpentyl (1-methylethyl)-
carbamate,B.
5-methyl-5-propyl-1,3-dioxan-2-one,C.
2-methyl-2-propylpropane-1,3-diol, D.2-methyl-2-propylpropane-1,3-diyl dicarbamate (meprobamate).
04/2010:2360corrected 7.0CARMELLOSE
Carmellosum DEFINITION
Polycarboxymethylether of cellulose.
CHARACTERS
Appearance :white or almost white powder,hygroscopic.
Solubility
:practically insoluble in anhydrous ethanol.It swells
with water to form a suspension and becomes viscid in 1M
sodium hydroxide.IDENTIFICATION
A.pH (2.2.3):3.5to 5.0.
Suspend 1.0g in 100mL of water R .
B.Infrared absorption spectrophotometry (2.2.24).
Comparison :carmellose CRS .
TESTS
Chlorides :maximum 0.36per cent.
Shake 0.8g with 50mL of water R ,dissolve in 10mL of 1M sodium
hydroxide and
dilute to 100mL with water R .Heat
on a
water-bath
a mixture of 10mL of dilute nitric acid R and
20mL of this solution until a flocculent precipitate is produced.Cool,centrifuge and take out the supernatant liquid.Wash
the
precipitate
with 3quantities,each of 10mL,of water R ,
centrifuging each https://www.360docs.net/doc/048642111.html,bine the supernatant liquid and the
washings and dilute to 100mL with water R .To 25mL of this solution
add 6mL of dilute nitric
acid R and dilute to 50mL
with water R (test solution).Prepare the reference solution with 0.40mL of 0.01M hydrochloric acid .Add 1mL of silver nitrate solution
R2to the test solution and the reference
solution.Allow to stand protected from light for 5min.Any opalescence in the test solution is not more intense than that in the reference solution.
Sulfates :maximum 0.72per cent.
Shake 0.40g with 25mL of water R ,dissolve in 5mL of 1M sodium hydroxide and add 20mL of water R .Heat this
solution with 2.5mL of hydrochloric acid R in a water-bath
until a flocculent precipitate is produced.Cool,centrifuge,and take out the supernatant liquid.Wash the precipitate with 3quantities,each of 10mL,of water R ,centrifuging each time.
Combine the supernatant liquid and the washings,and dilute to
100mL with water R .Filter,and discard the first 5mL of the filtrate.To 25mL of the filtrate add 1mL of dilute hydrochloric acid R and dilute to 50mL with water R (test solution).Prepare the reference solution with 1.5mL of 0.005M sulfuric acid .Add 2mL of a
120
g/L solution
of barium
chloride
R to
the test solution and the reference solution.Mix and allow to stand for 10min.The white turbidity produced in the test solution is not thicker than that in the reference solution.
Heavy metals :maximum 20ppm.
Place 1.0g in a quartz or porcelain crucible.Cover loosely with
a lid and carbonise by gentle ignition.Cool and add 2mL of nitric acid R and 5drops of
sulfuric
acid
R .Heat cautiously
until white fumes are no longer evolved and incinerate by
ignition at 500-600°C.Cool and add 2mL of hydrochloric acid R .Evaporate to dryness on a water-bath.Moisten the
1588See the information section on general monographs (cover pages)
EUROPEAN PHARMACOPOEIA 7.0Carmellose
sodium residue with 3drops of hydrochloric acid R ,add 10mL of hot water R and heat for 2min.Add 1drop of phenolphthalein solution R1,add dilute ammonia R1dropwise until the solution develops a pale red colour.Add 2mL of dilute acetic acid R ,filter if necessary,and wash with 10mL of water R .
Transfer the filtrate and washings to a test-tube,and dilute to 50mL with water R (test solution).Prepare the reference solution as follows:evaporate a mixture of 2mL of nitric acid R ,5drops of sulfuric acid R and 2mL of hydrochloric acid
R on
a water-bath,then evaporate to dryness on a sand-bath.Moisten the residue with 3drops of hydrochloric acid R .Proceed as described for the test solution,then add 2.0mL of lead standard solution (10ppm Pb)R and dilute to 50mL with water R .Add 0.1mL of sodium sulfide solution R1to the test solution and the reference solution and allow to stand for 5min.The colour of the test solution is not more intense than that of the reference solution.Loss on drying (2.2.32):maximum 8.0per cent,determined on 1.000g by drying in an oven at 105°C for 4h.Sulfated ash (2.4.14):maximum 1.5per cent,determined on 1.0g.STORAGE In an airtight container.01/2008:0886corrected 6.0CARMELLOSE CALCIUM Carmellosum calcicum [9050-04-8]DEFINITION Calcium salt of a partly O -carboxymethylated cellulose.CHARACTERS
Appearance :white or yellowish-white powder,hygroscopic
after drying.Solubility :practically insoluble in acetone,in alcohol and in
toluene.It swells with water to form a suspension.IDENTIFICATION A.Shake 0.1g thoroughly with 10mL of water R .Add 2mL of dilute sodium hydroxide solution R and allow to stand for 10min (solution A).Dilute 1mL of solution A to 5mL
with water R .To 0.05mL add 0.5mL of a 0.5g/L solution of chromotropic acid,sodium salt R in a 75per cent m/m solution of sulfuric acid R and heat on a water-bath for 10min.A reddish-violet colour develops.B.Shake 5mL of solution A obtained in identification test A with 10mL of acetone R .A white,flocculent precipitate is produced.C.Shake 5mL of solution A obtained in identification test A
with 1mL of ferric chloride solution R1.A brown,flocculent
precipitate is formed.D.Ignite 1g and dissolve the residue in a mixture of 5mL
of acetic acid R and 10mL of water R .Filter if necessary and boil the filtrate for a few minutes.Cool and neutralise with dilute ammonia R1.The solution gives reaction (a)of calcium (2.3.1).TESTS Solution S .Shake 1.0g with 50mL of distilled water R ,add 5mL of dilute sodium hydroxide solution R and dilute to 100mL with distilled water R .Alkalinity .Shake 1.0g thoroughly with 50mL of carbon dioxide-free water R and add 0.05mL of phenolphthalein solution R .No red colour develops.
Chlorides (2.4.4):maximum 0.36per cent.
Heat 28mL of solution S with 10mL of dilute nitric acid R on
a water-bath until a flocculent precipitate is produced.
Cool,centrifuge and separate the supernatant liquid.Wash the precipitate with 3quantities,each of 10mL,of water R ,centrifuging
each time.
Combine
the
supernatant
liquid
and
the
washings
and dilute to 100mL with water R .To 25mL add 6mL of dilute nitric acid R and dilute to 50mL with water R .
Dilute 10mL of the solution to 15mL with water R .Sulfates (2.4.13):maximum 1per cent.
Heat 20mL of solution S with 1mL of hydrochloric acid R on a water-bath
until
a flocculent
precipitate
is produced.
Cool,
centrifuge and separate the supernatant liquid.Wash the precipitate with 3quantities,each of 10mL,of distilled water R ,
centrifuging
each
time.
Combine the
supernatant
liquid
and the
washings
and dilute to 100mL with distilled water R .To 25mL
add 1mL of dilute hydrochloric acid R and dilute to 50mL with distilled water R .
Heavy metals (2.4.8):maximum 20ppm.
1.0g complies with test D.Prepare the reference solution using 2mL of lead standard solution (10ppm Pb)R .
Loss
on drying (2.2.32):maximum 10.0per cent,determined
on 1.000g by drying in an oven at 105°C for 4h.Sulfated ash (2.4.14):10.0per cent to 20.0per cent,determined
on 1.0g in a platinum crucible.STORAGE
In an airtight container.
01/2008:0472corrected 6.0CARMELLOSE SODIUM
Carmellosum natricum
[9004-32-4]
DEFINITION
Carmellose
sodium (carboxymethylcellulose sodium)is the sodium salt of a partly O -carboxymethylated cellulose.It contains
not less than 6.5per cent and not more than 10.8per cent of sodium (Na),calculated with reference to the dried substance.CHARACTERS
A
white or
almost white,
granular
powder,
hygroscopic after
drying,practically insoluble in acetone,in ethanol and in
toluene.It is easily dispersed in water giving colloidal solutions.IDENTIFICATION
A.To 10mL of solution S (see Tests)add 1mL of copper sulfate solution R .A blue,cotton-like precipitate is formed.
B.Boil 5mL of solution S for a few minutes.No precipitate
is formed.
C.The solution prepared from the sulfated ash in the test for heavy metals gives the reactions of sodium (2.3.1).
TESTS
Solution
S .Sprinkle a quantity of the substance to be examined equivalent to 1.0g of the dried substance onto 90mL of carbon dioxide-free
water
R at
40°C to 50°C stirring vigorously.
Continue stirring until a colloidal solution is obtained,cool and
dilute to 100mL with carbon dioxide-free water R .General Notices (1)apply to all monographs and other texts 1589