一水葡萄糖(EP)
Glucose monohydrate EUROPEAN PHARMACOPOEIA
7.0CHARACTERS Appearance :white or almost white,slightly hygroscopic powder or granules.Solubility :freely soluble in water.IDENTIFICATION A.Dissolve 0.1g in 2.5mL of water R and heat with 2.5mL of cupri-tartaric solution R .A red precipitate is formed.B.Dip,for 1s,a suitable stick with a reactive pad containing glucose-oxidase,peroxidase and a hydrogen-donating substance,such as tetramethylbenzidine,in a 5g/L solution of the substance to be examined.Observe the colour of the reactive pad;within 60s the colour changes from yellow to green or blue.C.It is a powder or granules.D.Dextrose equivalent (see Tests).TESTS Solution S .Dissolve 12.5g in carbon dioxide-free water R and dilute to 50.0mL with the same solvent.pH (2.2.3):4.0to 7.0.Mix 1mL of a 223.6g/L solution of potassium chloride R and 30mL of solution S.Sulfur dioxide (2.5.29):maximum 20ppm.
Heavy metals (2.4.8):maximum 10ppm.Dilute 4mL of solution S to 30mL with water R .The
solution complies with test E.Prepare the reference solution using 10mL of lead standard solution (1ppm Pb)R .Loss on drying (2.2.32):maximum 6.0per cent,determined on
10.00g by drying in an oven at 105°C.Sulfated ash (2.4.14):maximum 0.5per cent,determined on
1.0g.Dextrose equivalent (DE):within 10per cent of the nominal value.Weigh an amount of the substance
to be examined
equivalent
to 2.85-3.15g of reducing carbohydrates,calculated as dextrose equivalent,into a 500mL volumetric flask.Dissolve in water R and dilute to 500.0mL with the same solvent.Transfer the solution to a 50mL burette.Pipette 25.0mL of cupri-tartaric solution R into a 250mL flask and add 18.5mL of the test solution from the burette,mix and add a few
glass beads.
Place the
flask
on
a hot plate,
previously
adjusted so that the solution begins to boil after 2min ±15s.Allow to boil for exactly 120s,add 1mL of a 1g/L solution of methylene blue R and titrate with the test solution (V 1)until
the blue colour disappears.Maintain the solution at boiling throughout the titration.Standardise the cupri-tartaric solution using a 6.00g/L solution of glucose R (V 0).
Calculate the dextrose equivalent using the following expression:V 0=total volume of glucose standard solution,in millilitres;V 1=total volume of test solution,in millilitres;M =mass of the sample,in grams;D =percentage content of dry matter in the substance.Microbial contamination TAMC:acceptance criterion 103CFU/g (2.6.12).TYMC:acceptance criterion 102CFU/g (2.6.12).Absence of Escherichia coli (2.6.13).Absence of Salmonella (2.6.13).LABELLING
The label states the dextrose equivalent (DE)(=nominal value).FUNCTIONALITY-RELATED CHARACTERISTICS
This section provides information on characteristics that are recognised as being relevant control parameters for one or
more
functions of the substance when used as an excipient (see chapter 5.15).This section is a non-mandatory part of the
monograph and it is not necessary to verify the characteristics
to demonstrate compliance.Control of these characteristics
can however contribute to the quality of a medicinal product by improving the consistency of the manufacturing process and
the performance of the medicinal product during use.Where control methods are cited,they are recognised as being
suitable
for
the purpose,but other methods can also be used.
Wherever results for a particular characteristic are reported,
the control method must be indicated.The
following characteristics may be relevant for spray-dried liquid glucose used as filler or binder for wet granulation.
Dextrose equivalent (see Tests).
Particle-size distribution (2.9.31or 2.9.38).
01/2008:0178corrected 6.3GLUCOSE MONOHYDRATE Glucosum
monohydricum
C 6H 12O 6,H 2O M r 198.2[5996-10-1]
DEFINITION
(+)-D -Glucopyranose monohydrate.
CHARACTERS
Appearance :white or almost white,crystalline powder.
It has a sweet taste.
Solubility
:freely soluble in water,sparingly soluble in ethanol
(96per cent).IDENTIFICATION
A.Specific optical rotation (see Tests).
B.Thin-layer chromatography (2.2.27).
Solvent mixture :water R ,methanol R (2:3V/V ).
Test
solution .Dissolve 10mg of the substance to be examined in the solvent mixture and dilute to 20mL with the solvent mixture.
Reference solution (a).Dissolve 10mg of glucose CRS in the
solvent mixture and dilute to 20mL with the solvent mixture.Reference solution (b).Dissolve 10mg each of fructose CRS ,glucose CRS ,lactose CRS and sucrose CRS in the solvent
mixture and dilute to 20mL with the solvent mixture.
Plate :TLC silica gel G plate R .
Mobile phase :water R ,methanol R ,anhydrous acetic acid R ,ethylene chloride R (10:15:25:50V/V/V/V );measure the volumes accurately since a slight excess of water produces cloudiness.
Application :2μL;thoroughly dry the points of application.Development A :over a path of 15cm.
Drying A :in a current of warm air.
Development B :immediately,over a path of 15cm,after renewing the mobile phase.2104See the information section on general monographs (cover pages)
EUROPEAN PHARMACOPOEIA 7.0Glutamic
acid Drying B :in a current of warm air.Detection :spray with a solution of 0.5g of thymol R in a mixture of 5mL of sulfuric acid R and 95mL of ethanol (96per cent)R ;heat at 130°C for 10min.System suitability :reference solution (b):—the chromatogram shows 4clearly 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 0.1g in 10mL of water R .Add 3mL of cupri-tartaric solution R and heat.A red precipitate is formed.TESTS Solution S .Dissolve 10.0g in distilled water R and dilute to
100mL with the same solvent.Appearance of solution .The solution is clear (2.2.1)and not more intensely coloured than reference solution BY 7(2.2.2,Method II ).
Dissolve 10.0g in 15mL of water R .Acidity or alkalinity .Dissolve 6.0g in 25mL of carbon
dioxide-free water R and add 0.3mL of phenolphthalein solution R .The solution is colourless.Not more than 0.15mL
of 0.1M sodium hydroxide is required to change the colour
of the indicator to pink.Specific optical rotation (2.2.7):+52.5to +53.3(anhydrous substance).Dissolve 10.0g in 80mL of water R ,add 0.2mL of dilute ammonia R1,allow to stand for 30min and dilute to 100.0mL with water R .Foreign sugars,soluble starch,dextrins .Dissolve 1.0g by
boiling in 30mL of ethanol (90per cent V/V)R .Cool;the
appearance of the solution shows no change.Sulfites :maximum 15ppm,expressed as SO 2.
Test solution .Dissolve 5.0g in 40mL
of
water
R ,add 2.0mL of
0.1M sodium hydroxide and dilute to 50.0mL with water R .To 10.0mL of the solution,add 1mL of a 310g/L solution of hydrochloric acid R ,2.0mL of decolorised fuchsin solution R1and 2.0mL of a 0.5per cent V/V solution of formaldehyde R .Allow to stand for 30min.Reference solution .Dissolve
76mg of sodium metabisulfite R
in water R and dilute to 50.0mL with the same solvent.Dilute 5.0mL of this solution to 100.0mL with water R .To 3.0mL of this solution add 4.0mL of 0.1M sodium hydroxide and dilute to 100.0mL with water R .Immediately add to 10.0mL
of this
solution 1mL of a 310g/L solution of hydrochloric acid R ,2.0mL of decolorised fuchsin solution R1and 2.0mL of a 0.5per cent V/V solution of formaldehyde R .Allow to stand for 30min.Measure the absorbance (2.2.25)of the
2solutions at the
absorption maximum at 583nm using for both measurements a solution prepared in the same manner using 10.0mL of water R as the compensation liquid.The absorbance of the test solution is not greater than that of the reference solution.Chlorides (2.4.4):maximum 125ppm.Dilute 4mL of solution S to 15mL with water R .Sulfates (2.4.13):maximum 200ppm.Dilute 7.5mL of solution S to 15mL with distilled water R .Arsenic (2.4.2,Method A ):maximum 1ppm,determined on 1.0g.Barium .To 10mL of solution S add 1mL of dilute sulfuric
acid R .When examined immediately and after 1h,any
opalescence in the solution is not more intense than that in a
mixture of 1mL of distilled water R and 10mL of solution S.Calcium (2.4.3):maximum 200ppm.
Dilute 5mL of solution S to 15mL with distilled water R .Lead (2.4.10):maximum 0.5ppm.
Water
(2.5.12):7.0per cent to 9.5per cent,determined on 0.50g.Sulfated ash :maximum 0.1per cent.
Dissolve 5.0g in 5mL of water R ,add 2mL of sulfuric acid R ,evaporate
to dryness on a water-bath and ignite to constant mass.If necessary,repeat the heating with sulfuric acid R .Pyrogens
(2.6.8).If intended for use in the manufacture of large-volume parenteral preparations without a further appropriate procedure for
the removal of pyrogens,
the
competent authority may require that it comply with the test for pyrogens.Inject per kilogram of the rabbit’s mass 10mL of
a solution in water for injections R containing 55mg of the substance to be examined per millilitre.01/2008:0750corrected 6.0
GLUTAMIC ACID
Acidum
glutamicum
C
5H 9NO 4M r 147.1[56-86-0]DEFINITION
Glutamic acid contains not less than 98.5per cent
and not more than the equivalent of 100.5per cent of (2S )-2-aminopentanedioic acid,calculated with reference to the dried substance.
CHARACTERS
A
white or almost white,crystalline powder or colourless crystals,freely soluble in boiling water,slightly soluble in cold water,
practically insoluble in acetic acid,in acetone and in alcohol.IDENTIFICATION
First identification:A,B .
Second identification:A,C,D .
A.Specific optical rotation (see Tests).
B.Examine
by infrared absorption spectrophotometry (2.2.24),comparing with the spectrum obtained with glutamic acid
CRS .Examine the substances prepared as discs.If the
spectra obtained show differences,dissolve the substance to
be
examined and the reference substance separately in the minimum quantity of water R ,evaporate to dryness at 60°C
and record new spectra using the residues.
C.Examine the chromatograms obtained in the test for ninhydrin-positive
substances.
The
principal
spot
in the
chromatogram
obtained with test solution (b)is similar in position,colour and size to the principal spot in the
chromatogram obtained with reference solution (a).
D.To 2.0mL of solution S (see Tests)add 0.1mL of
phenolphthalein
solution R and 3.0mL to 3.5mL of 1M
sodium hydroxide to change the colour of the indicator to
red.Add a mixture of 3mL of formaldehyde solution R ,3mL of carbon dioxide-free water R and 0.1mL of phenolphthalein solution R ,to which sufficient 1M sodium hydroxide
has been added to produce a pink colour.The
solution is decolourised.Add 1M sodium hydroxide until
a red colour is produced.The total volume of 1M sodium hydroxide used is 4.0mL to 4.7mL.
TESTS Solution S .Dissolve 5.00g in 1M hydrochloric acid with gentle heating,and dilute to 50.0mL with the same acid.General Notices (1)apply to all monographs and other texts 2105