Cisplatin EUROPEAN PHARMACOPOEIA
6.0
01/2008:0599corrected 6.0CISPLATIN
Cisplatinum蜂蜜柚子茶的正确做法
[PtCl 2(NH 3)2]M r 300.0[15663-27-1]
DEFINITION Cisplatin contains not less than 97.0per cent and not more than the equivalent of 102.0per cent of cis -diamminedi-chloroplatinum (II).CHARACTERS
A yellow powder or yellow or orange-yellow crystals,slightly soluble in water,sparingly soluble in dimethylformamide,
practically insoluble in alcohol.
It decompos with blackening at about 270°C.
Carry out identification test B,the tests (except that for
silver)and the assay protected from light .
IDENTIFICATION First identification:A,B .
Second identification :B,C .A.Examine by infrared absorption spectrophotometry (2.2.24),comparing with the spectrum obtained with
cisplatin CRS .Examine the substances prepared as discs
in potassium bromide R .
B.Examine the chromatograms obtained in the test
for related substances.The principal spot in the
chromatogram obtained with test solution (a)is similar
in position,colour and size to the principal spot in the
chromatogram obtained with reference solution (a).
C.Add 50mg to 2ml of dilute sodium hydroxide solution R in a glass dish.Evaporate to dryness.Dissolve the residue
in a mixture of 0.5ml of nitric acid R and 1.5ml of
hydrochloric acid R .Evaporate to dryness.The residue癌组词
is orange.Dissolve the residue in 0.5ml of water R and
add 0.5ml of ammonium chloride solution R .A yellow,
crystalline precipitate is formed.TESTS
Solution S1.Dissolve 25mg in a 9g/l solution of sodium chloride R prepared with carbon dioxide-free water R and dilute to 25ml with the same solvent.Solution S2.Dissolve 0.20g in dimethylformamide R and dilute to 10ml with the same solvent.Appearance of solution S1.Solution S1is clear (2.2.1)and
黑风山答题
not more intenly coloured than reference solution GY 5(2.2.2,Method II ).Appearance of solution S2.Solution S2is clear (2.2.1).
pH (2.2.3).The pH of solution S1,measured immediately
after preparation,is 4.5to 6.0.
Related substances .Examine by thin-layer chromatography (2.2.27),using cellulo for chromatography R1as the coating substance.Activate the plate by heating at 150°C for 1h.Test solution (a).Dilute 1ml of solution S2to 10ml with
dimethylformamide R .
Test solution (b).U solution S2.Reference solution (a).Dissolve 10mg of cisplatin CRS in 5ml of dimethylformamide R .
Reference solution (b).Dilute 1ml of solution S2to 50ml with dimethylformamide R .Apply parately to the plate 2.5µl of test solution (a),2.5µl of reference solution (a),5µl of test solution (b)and 5µl of reference solution (b).Develop over a path of 15cm using a mixture of 10volumes of acetone R and 90volumes of dimethylformamide R .Allow the plate to dry in air and spray with a 50g/l solution of stannous chloride R in a mixture of equal volumes of dilute hydrochloric acid R and
water R .After 1h,the chromatogram obtained with test
solution (b)shows no spot with an R F value less than that of the principal spot and any spot with an R F value greater than
that of the principal spot is not more inten than the spot in the chromatogram obtained with reference solution (b).Silver .Not more than 2.5×102ppm of Ag,determined by atomic absorption spectrometry (2.2.23,Method I ).
Test solution .Dissolve 0.100g of the substance to be examined in 15ml of nitric acid R ,heating to 80°C.Cool
and dilute to 25.0ml with water R .Reference solutions .To suitable volumes (10ml to 30ml)of silver standard solution (5ppm Ag)R add 50ml of nitric acid R and dilute to 100.0ml with water R .
Measure the absorbance at 328nm using a silver hollow-cathode lamp as source of radiation,a fuel-lean
air-acetylene flame and,preferably,a spectral slit width of
0.5nm.Carry out a blank determination.ASSAY Examine by liquid chromatography (2.2.29).Test solution .Dissolve 50.0mg of the substance to be
examined in a 9g/l solution of sodium chloride R and dilute
to 100.0ml with the same solvent.
Reference solution .Dissolve 50.0mg of cisplatin CRS in a
9g/l solution of sodium chloride R and dilute to 100.0ml
with the same solvent.
The chromatographic procedure may be carried out using : a column 0.25m long and 4.6mm in internal diameter
packed with strong-anion-exchange silica gel for chromatography R (10µm), as mobile pha at a flow rate of 1.2ml/min a mixture of 10volumes of a 9g/l solution of sodium chloride R and 90volumes of methanol R , as detector a spectrophotometer t at 220nm.
U a sample loop.Inject parately 20µl of the test solution and 20µl of the reference solution.
独一无二的英文昵称STORAGE Store in an airtight container,protected from light.01/2008:0455
corrected 6.0CITRIC ACID,ANHYDROUS Acidum citricum
anhydricum C 6H 8O 7M r 192.1[77-92-9]DEFINITION 2-Hydroxypropane-1,2,3-tricarboxylic acid.1554
See the information ction on general monographs (cover pages)
EUROPEAN PHARMACOPOEIA 6.0Citric acid
monohydrate
Content :99.5per cent to 100.5per cent (anhydrous substance).
CHARACTERS
Appearance :white or almost white,crystalline powder,colourless crystals or granules.
Solubility :very soluble in water,freely soluble in ethanol (96per cent).
mp:about 153°C,with decomposition.
IDENTIFICATION
不可触摸First identification:B,E .
Second identification :A,C,D,E .
A.Dissolve 1g in 10ml of water R .The solution is strongly acidic (2.2.4).
B.Infrared absorption spectrophotometry (2.2.24).
Preparation :dry the substance to be examined and the reference substance at 100-105°C for 2h.Comparison :anhydrous citric acid CRS .
C.Add about 5mg to a mixture of 1ml of acetic anhydride R and 3ml of pyridine R .A red colour develops.
D.Dissolve 0.5g in 5ml of water R ,neutrali using 1M sodium hydroxide (about 7ml),add 10ml of
怎么按摩前列腺calcium chloride solution R and heat to boiling.A white precipitate is formed.E.Water (e Tests).
TESTS
李学玲Appearance of solution .The solution is clear (2.2.1)and not more intenly coloured than reference solution Y 7,BY 7or GY 7(2.2.2,Method II ).
最佳团队奖颁奖词Dissolve 2.0g in water R and dilute to 10ml with the same solvent.
Readily carbonisable substances .To 1.0g in a cleaned test tube add 10ml of sulphuric acid R and immediately heat the mixture in a water-bath at 90±1°C for 60min.Cool rapidly immediately afterwards.The solution is not more intenly coloured than a mixture of 1ml of red primary solution and 9ml of yellow primary solution (2.2.2,Method I ).
Oxalic acid :maximum 360ppm,calculated as anhydrous oxalic acid.
Dissolve 0.80g in 4ml of water R .Add 3ml of hydrochloric acid R and 1g of zinc R in granules.Boil for 1min.Allow to stand for 2min.Transfer the supernatant liquid to a test-tube containing 0.25ml of a 10g/l solution of phenylhydrazine hydrochloride R and heat to boiling.Cool rapidly,transfer to a graduated cylinder and add an equal volume of hydrochloric acid R and 0.25ml of a 50g/l solution of potassium ferricyanide R .Shake and allow to stand for 30min.Any pink colour in the solution is not more inten than that in a standard prepared at the same time in the same manner using 4ml of a 0.1g/l solution of oxalic acid R .
Sulphates (2.4.13):maximum 150ppm.
Dissolve 2.0g in distilled water R and dilute to 30ml with the same solvent.
Aluminium (2.4.17):maximum 0.2ppm,if intended for u in the manufacture of dialysis solutions.
Prescribed solution .Dissolve 20g in 100ml of water R and add 10ml of acetate buffer solution pH 6.0R .
Reference solution .Mix 2ml of aluminium standard solution (2ppm Al)R ,10ml of acetate buffer solution pH 6.0R and 98ml of water R .
Blank solution .Mix 10ml of acetate buffer solution pH 6.0R and 100ml of water R .
Heavy metals (2.4.8):maximum 10ppm.
Dissolve 5.0g in veral portions in 39ml of dilute sodium hydroxide solution R and dilute to 50ml with distilled water R .12ml of the solution complies with test A.
Prepare the reference solution using lead standard solution (1ppm Pb)R .
Water (2.5.12):maximum 1.0per cent,determined on 2.000g.
Sulphated ash (2.4.14):maximum 0.1per cent,determined on 1.0g.
Bacterial endotoxins (2.6.14):less than 0.5IU/mg,if intended for u in the manufacture of parenteral dosage forms without a further appropriate procedure for the removal of bacterial endotoxins.
ASSAY
Dissolve 0.550g in 50ml of water R .Titrate with 1M sodium hydroxide ,using 0.5ml of phenolphthalein solution R as indicator.
1ml of 1M sodium hydroxide is equivalent to 64.03mg of C 6H 8O 7.
LABELLING
The label states,where applicable,that the substance is intended for u in the manufacture of dialysis solutions.
01/2008:0456corrected 6.0
CITRIC ACID MONOHYDRATE Acidum citricum
monohydricum
C 6H 8O 7,H 2O M r 210.1
[5949-29-1]
DEFINITION
2-Hydroxypropane-1,2,3-tricarboxylic acid monohydrate.Content :99.5per cent to 100.5per cent (anhydrous substance).
CHARACTERS
Appearance :white or almost white,crystalline powder,colourless crystals or granules,efflorescent.
Solubility :very soluble in water,freely soluble in ethanol (96per cent).
IDENTIFICATION
First identification:B,E .
Second identification:A,C,D,E .
A.Dissolve 1g in 10ml of water R .The solution is strongly acidic (2.2.4).
B.Infrared absorption spectrophotometry (2.2.24).
Preparation :dry the substance to be examined and the reference substance at 100-105°C for 2h.Comparison :citric acid monohydrate CRS .
C.Add about 5mg to a mixture of 1ml of acetic anhydride R and 3ml of pyridine R .A red colour develops.
D.Dissolve 0.5g in 5ml of water R ,neutrali using 1M sodium hydroxide (about 7ml),add 10ml of
calcium chloride solution R and heat to boiling.A white precipitate is formed.E.Water (e Tests).
General Notices (1)apply to all monographs and other texts
1555
