Trometamol EUROPEAN PHARMACOPOEIA
7.0Water (2.5.12):maximum 1.0per cent,determined on 1.000g.Open the titration vesl,introduce the substance to be examined directly into the previously titrated solvent.Stopper the flask immediately.Sulfated ash (2.4.14):maximum 0.1per cent,determined on
1.0g.Do not carry out the initial heating on a water-bath.ASSAY Dissolve 1.200g in 75mL of carbon dioxide-free water R .Add 0.3mL of methyl red solution R .Titrate with 1M hydrochloric acid .1mL of 1M hydrochloric acid is equivalent to 0.149g of C 6H 15NO 3.STORAGE In an airtight container,protected from light.IMPURITIES Specified impurities:A,B,
C.A.2-aminoethanol
(ethanolamine),B.2,2′-iminodiethanol
(diethanolamine),C.2,2′-(nitrosoimino)diethanol (N -nitrosodiethanolamine).01/2008:1053corrected 6.0TROMETAMOL
Trometamolum C 4H 11NO 3M r 121.1
[77-86-1]DEFINITION Trometamol contains not less than 99.0
per cent and not more than the equivalent of 100.5per cent of aminomethylidynetri(methanol),calculated with reference to the dried substance.CHARACTERS A white or almost white,crystalline
powder,or colourless crystals,freely soluble in water,sparingly soluble in alcohol,very slightly soluble in ethyl acetate.IDENTIFICATION First identification:B,C .Second identification:A,B,D .A.Solution S (e Tests)is strongly alkaline (2.2.4).
B.Melting point (2.2.14):168°C to 174°
C.
C.Examine by infrared absorption spectrophotometry (2.2.24),comparing with the spectrum obtained with trometamol CRS .
D.Examine
the chromatograms obtained in the test for related 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).TESTS
Solution S .Dissolve 2.5g in carbon dioxide-free water R and dilute to 50mL with the same solvent.
Appearance of solution .Solution S is clear (2.2.1)and colourless (2.2.2,Method II ).azo
pH (2.2.3).The pH of freshly prepared solution S is 10.0to 11.5.
Related
substances .Examine by thin-layer
chromatography
(
2.2.27),using silica gel G R as the coating substance.Wash
the plate with methanol R before applying the solutions.Test solution (a).Dissolve 0.20g in 1mL of家长怎样与孩子沟通
water R ,with heating,and dilute to 10mL with methanol R .Test solution (b).Dilute 1mL of test solution (a)to 10mL with
methanol R .Reference
solution (a).Dissolve 20mg of trometamol CRS in
methanol R and dilute to 10mL with the same solvent.Reference solution (b).Dilute 1mL of test solution (a)to
指示牌英文100mL with methanol R .Apply
to the plate 10μL of each solution.Develop over a path of
10cm using a mixture of 10volumes of dilute ammonia R1and 90volumes of 2-propanol R .Dry the plate at 100°C to 105°C.
Spray with a 5g/L solution of potassium permanganate R in
a 10g/L solution of sodium carbonate R .After about 10min examine in
daylight.
Any spot
in the
chromatogram obtained
with test solution (a),apart from the principal spot,is not more
inten than the spot in the chromatogram obtained with reference solution (b)(1.0per cent).
Chlorides (2.4.4).To 10mL of solution S add
2.5
mL of dilute
nitric
acid R and dilute to 15mL with water R .The solution complies with the limit test for chlorides (100ppm).Heavy
metals
复式记账
(2.4.8).Dissolve 2.0g in 10mL of water R .
Neutrali the solution with hydrochloric acid R1and dilute to
20mL with water R .12mL of the solution complies with limit
test A for heavy metals (10ppm).Prepare the standard using lead standard solution (1ppm Pb)R .
胡萝卜的英文单词Iron (2.4.9).Dissolve 1.0g in water R and dilute to 10mL with the same solvent.The solution complies with the limit test for iron (10ppm).
Loss on drying (2.2.32).Not more than 0.5per cent,determined
on 1.000g by drying in an oven at 105°C.Sulfatedmelody意思
ash (2.4.14).Not more than 0.1per cent,determined on 1.0g.Bacterial endotoxins (2.6.14):less than 0.03IU/mg,if intended for u in the manufacture of parenteral preparations without
a further appropriate procedure for the removal of bacterial
endotoxins.
ASSAY
Dissolve 0.100g in 20mL of water R .Add 0.2mL of methyl red
solution R .Titrate with 0.1M hydrochloric acid until the
colour changes from yellow to red.1mL of 0.1M hydrochloric acid is equivalent to 12.11mg of C 4H 11NO 3.
IMPURITIES
A.nitromethylidynetri(methanol).
3150See the information ction on general monographs (cover pages)
EUROPEAN PHARMACOPOEIA 7.0
Tropicamide
01/2011:1159TROPICAMIDE
Tropicamidum C 17H 20N 2O 2M r 284.4[1508-75-4]DEFINITION (2RS )-N -Ethyl-3-hydroxy-2-phenyl-N -(pyridin-4-ylmethyl)propa-namide.Content :99.0per cent to 101.0per cent (dried substance).CHARACTERS Appearance :white or almost white,crystalline powder.Solubility :slightly soluble in water,freely soluble in ethanol (96per cent)and in methylene chloride.IDENTIFICATION
First identification:C .
Second identification:A,B,D,E .从句讲解
老友记第九季
A.Melting point (2.2.14):95°C to 98°C.
B.Ultraviolet and visible absorption spectrophotometry (2.2.25).Test solution .Dissolve 20.0mg in 0.1M hydrochloric acid and dilute to 50.0mL with the same acid.Dilute 2.0mL of this solution to 20.0mL with 0.1M hydrochloric acid .Spectral range :230-350nm.Absorption maximum :at 254nm.Specific absorbance at the absorption maximum :170to 190.
C.Infrared absorption spectrophotometry (2.2.24).Comparison :tropicamide CRS .
foreignersD.Thin-layer chromatography (2.2.27).Test solution .Dissolve 10mg of the substance to be examined in methylene chloride R and dilute to 10mL with the same solvent.Reference solution .Dissolve 10mg
of tropicamide CRS in methylene chloride R and dilute to 10mL with the same solvent.Plate :TLC silica gel F 254plate R .Mobile pha :concentrated ammonia R ,methanol R ,methylene chloride R (0.5:5:95V/V/V ).Application :10μL.Development :over 2/3of the plate.Drying :in air.Detection :examine in ultraviolet light at 254nm.Results :the principal spot in the chromatogram obtained with the test solution is similar in position and size to the spot in the chromatogram obtained with the reference solution.
E.Dissolve about 5mg in 3mL of a mixture of 9mL of acetic anhydride R ,1mL of acetic acid R and 0.1g of citric acid R .Heat on a water-bath for 5-10min.A reddish-yellow colour is produced.TESTS Appearance of solution .The solution is clear (2.2.1)and colourless (2.2.2,Method II ).Dissolve 0.1g in ethanol (96per cent)R and dilute to 10mL with the same solvent.Optical rotation (2.2.7):−0.1°to +0.1°.
Dissolve 2.5g in anhydrous ethanol R and dilute to 25.0mL with the same solvent.Related substances .Liquid chromatography (2.2.29).Test solution .Dissolve 50.0mg of the substance to be examined in 3mL of acetonitrile R1and dilute to 50.0mL with water for chromatography R .
Reference solution (a).Dilute 1.0mL of the test solution to 100.0mL with water for chromatography R .Dilute 1.0mL of this solution to 10.0mL with water for chromatography R .
Reference solution (b).Dissolve 5mg of 4-[(ethylami-no)methyl]pyridine R (impurity A),5.0mg of tropicamide impurity C CRS and 5.0mg of tropicamide impurity D CRS in 2mL of acetonitrile R1and dilute to 50.0mL with water for chromatography R .Dilute 1.0mL of this solution to 10.0mL with water for chromatography R .Reference solution (c).Dissolve 5mg of tropicamide for peak identification CRS (containing impurity B)in 1.0mL of acetonitrile R1and dilute to 10.0mL with water for chromatography R .Reference solution (d).To 1mL of reference solution (b)add 1mL of reference solution (c).Reference solution (e).Dilute 1.5mL of reference solution (b)to 10.0mL with water for chromatography R .Column :—size :l =0.15m,Ø=4.6mm;—stationary pha :end-capped octadecylsilyl silica gel for chromatography R (3μm);—temperature :40°C.
Mobile pha .Dissolve 0.135g of sodium dodecyl sulfate R and 3.4mL of phosphoric acid R in 950mL of water for chromatography R .Adjust to pH 3.0with strong sodium hydroxide solution R and dilute to 1000mL with water for chromatography R .Mix 73volumes of this solution with 27volumes of acetonitrile R1.Flow rate :0.8mL/min.Detection :spectrophotometer at 210nm and at 254nm.Injection :15μL.Run time :3times the retention time of tropicamide.Identification of impurities :u the chromatogram obtained with reference solution (c)to identify the peak due to impurity B;u the chromatogram obtained with reference solution (b)to identify the peaks due to impurities A,C and D.
Relative retention with reference to tropicamide (retention time =about 11min):impurity C =about 0.4;impurity A =about 0.5;impurity D =about 0.8;impurity B =about 2.3.
System suitability :reference solution (d):
—resolution at 210nm :minimum 2.0between the peaks due to impurities C and A;
—resolution at 210nm :minimum 2.0between the peaks due to impurities A and D.Limits :—correction factors :for the calculation of content,multiply the peak areas of the following impurities by the corresponding correction factor:impurity A =0.8;impurity B =0.6;—impurity B at 254nm :not more than 3times the area of the principal peak in the chromatogram obtained with reference solution (a)(0.3per cent);—impurity A at 254nm :not more than 1.5times the area of the principal peak in the chr
obd是什么意思omatogram obtained with reference solution (a)(0.15per cent);—impurity C at 210nm :not more than the area of the corresponding peak in the chromatogram obtained with reference solution (e)(0.15per cent);—impurity D at 210nm :not more than the area of the corresponding peak in the chromatogram obtained with reference solution (e)(0.15per cent);
General Notices (1)apply to all monographs and other texts 3151
