EUROPEAN PHARMACOPOEIA 7.0Dexamethasone
acetate
C.9-fluoro-11β,17,21-trihydroxy-16α-methylpregn-4-ene-3,20-
dione,
D.17,21-dihydroxy-16α-methyl-9β,11β-epoxypregna-1,4-diene-3,
20-dione,
E.17,21-dihydroxy-16α-methylpregna-1,4,9(11)-triene-3,20-
dione,
F.9-fluoro-11β,21-dihydroxy-16α-methylpregna-1,4-diene-3,20-
dione,G.9-fluoro-11β,17-dihydroxy-16α-methyl-3,20-dioxopregna-1,4-dien-21-yl acetate (dexamethasone
acetate),H.17-hydroxy-16α-methyl-3,20-dioxopregna-1,4,9(11)-trien-21-yl
acetate.
英语作文 我的梦想04/2010:0548DEXAMETHASONE ACETATE Dexamethasoni
acetas
C 24H 31FO 6M r 434.5[1177-87-3]DEFINITION
9-Fluoro-11β,17-dihydroxy-16α-methyl-3,20-dioxopregna-1,4-dien-21-yl acetate.
Content :97.0per cent to 103.0per cent (dried substance).CHARACTERS
Appearance :white or almost white,crystalline powder.Solubility :practically insoluble in water,freely soluble in ethanol (96per cent),slightly soluble in methylene chloride.It shows polymorphism (5.9).
IDENTIFICATION
First identification:B,C .
Second identification:A,C,D,E,F .
A.Dissolve 10.0mg in anhydrous ethanol R and dilute to 100.0mL with the same solvent.Place 2.0mL of this solution in a ground-glass-stoppered tube,add 10.0mL of phenylhydrazine-sulfuric acid solution R ,mix and heat in a water-bath at 60°C for 20min.Cool immediately.The absorbance (2.2.25)measured at the absorption maximum at 419nm is not less than 0.35.
B.Infrared absorption spectrophotometry (2.2.24).Comparison :dexamethasone acetate CRS .
If the spectra obtained in the solid state show differences,dissolve the substance to be examined and the reference substance parately in methylene chloride R ,evaporate to dryness and record new spectra using the residues.C.Thin-layer chromatography (2.2.27).
Solvent mixture :methanol R ,methylene chloride R (1:9V/V ).
Test solution .Dissolve 10mg of the substance to be
examined in the solvent mixture and dilute to 10mL with the solvent mixture.
Reference solution (a).Dissolve 20mg of dexamethasone
acetate CRS in the solvent mixture and dilute to 20mL with
the solvent mixture.
Reference solution (b).Dissolve 10mg of cortisone acetate R in reference solution (a)and dilute to 10mL with reference solution (a).
Plate :TLC silica gel F 254plate R .
Mobile pha :add a mixture of 1.2volumes of water R and 8volumes of methanol R to a mixture of 15volumes of
ether R and 77volumes of methylene chloride R .
Application :5μL.
Development :over 3/4of the plate.Drying :in air.
Detection A :examine in ultraviolet light at 254nm.
Results A :the principal spot in the chromatogram obtained with the test solution is similar in position and size to the principal spot in the chromatogram obtained with reference solution (a).Detection B :spray with alcoholic solution of sulfuric acid R ,heat at 120°C for 10min or until the spots appear,and allow to cool;examine in daylight and in ultraviolet light at 365nm.
Results B :the principal spot in the chromatogram obtained
with the test solution is similar in position,colour in daylight,
fluorescence in ultraviolet light at 365nm and size to the
principal spot in the chromatogram obtained with reference solution (a).System suitability :reference solution (b):
—the chromatogram shows 2clearly parated spots.D.Add about 2mg to 2mL of sulfuric acid R and shake to dissolve.Within 5min,a faint reddish-brown colour develops.Add this solution to 10mL of water R and mix.The colour is discharged and a clear solution remains.E.Mix about 5mg with 45mg of heavy magnesium oxide R
and ignite in a crucible until an almost white residue is obtained (usually less than 5min).Allow to cool,add 1mL of General Notices (1)apply to all monographs and other texts
1809
wmo
Dexamethasone acetate EUROPEAN PHARMACOPOEIA
7.0
water R,0.05mL of phenolphthalein solution R1and about 1mL of dilute hydrochloric acid R to render the solution colourless.Filter.To a freshly prepared mixture of0.1mL of alizarin S solution R and0.1mL of zirconyl nitrate
solution R,add1.0mL of the filtrate.Mix,allow to stand for5min and compare the colour of the solution with that of a blank prepared in the same manner.The test solution is yellow and the blank is red.
F.About10mg gives the reaction of acetyl(2.3.1).
naughty是什么意思TESTS
Specific optical rotation(2.2.7):+94to+99(dried substance). Dissolve0.250g in anhydrous ethanol R and dilute to25.0mL with the same solvent.
Related substances.Liquid chromatography(2.2.29).Carry out the test protected from light.
Test solution.Dissolve25mg of the substance to be examined in about4mL of acetonitrile R and dilute to10.0mL with water R.
Reference solution(a).Dissolve2mg of dexamethasone CRS (impurity A)and2mg of betamethasone acetate CRS (impurity D)in100.0mL of the mobile pha and sonicate for about10min(solution A).Mix6.0mL of the test solution and 1.0mL of solution A and dilute to10.0mL with the mobile pha.
Reference solution(b).Dilute1.0mL of the test solution to 100.0mL with the mobile pha.Dilute1.0mL of this solution to10.0mL with the mobile pha.
Reference solution(c).Dissolve the contents of a vial of dexamethasone acetate impurity E CRS in1.0mL of the mobile pha.
Column:
—size:l=0.25m,Ø=4.6mm;
—stationary pha:octadecylsilyl silica gel for
teenagechromatography R(5μm).
Mobile pha:mix380mL of acetonitrile R with550mL of water R and allow to equilibrate;dilute to1000.0mL with water R and mix again.
Flow rate:1mL/min.
Detection:spectrophotometer at254nm.
Injection:20μL.
Run time:2.5times the retention time of dexamethasone acetate.stricter
Identification of impurities:u the chromatogram obtained with reference solution(a)to identify the peaks due to impurities A and D;u the chromatogram obtained with reference solution(c)to identify the peak due to impurity E.
Relative retention with reference to dexamethasone acetate (retention time=about22min):impurity A=about0.4; impurity D=about0.9;impurity E=about1.2.
System suitability:reference solution(a):
—resolution:minimum3.3between the peaks due to impurity D and dexamethasone acetate.
Limits:
—impurity D:not more than3times the area of the principal peak in the chromatogram obtained with reference
solution(b)(0.3per cent);
—impurities A,E:for each impurity,not more than twice the area of the principal peak in the chromatogram obtained
with reference solution(b)(0.2per cent);
—unspecified impurities:for each impurity,not more than the area of the principal peak in the chromatogram obtained
with reference solution(b)(0.10per cent);—total:not more than5times the area of the principal peak in the chromatogram obtained with reference solution(b)
(0.5per cent);
—disregard limit:0.5times the area of the principal peak in the chromatogram obtained with reference solution(b)
(0.05per cent).
Loss on drying(2.2.32):maximum0.5per cent,determined on 0.500g by drying in vacuo in an oven at105°C.
ASSAY
Dissolve0.100g in ethanol(96per cent)R and dilute to 100.0mL with the same solvent.Dilute2.0mL of this solution to100.0mL with ethanol(96per cent)R.Measure the absorbance(2.2.25)at the absorption maximum at238.5nm. Calculate the content of C
24
H
31
FO
6
taking the specific absorbance to be357.
STORAGE
Protected from light.
IMPURITIES
Specified impurities:A,D,E.
Other detectable impurities(the following substances would, if prent at a sufficient level,be detected by one or other of the tests in the monograph.They are limited by the general acceptance criterion for other/unspecified impurities and/or by the general monograph Substances for pharmaceutical u (2034).It is therefore not necessary to identify the impurities for demonstration of compliance.See also5.10.Control of impurities in substances for pharmaceutical u):B,C,F,G,
H.
A.9-fluoro-11β,17,21-trihydroxy-16α-methylpregna-1,4-diene-3,
20-dione
(dexamethasone),
B.14-fluoro-11β,17-dihydroxy-16α-methyl-3,20-dioxopregna-1,4-
dien-21-yl
acetate,
C.9-fluoro-11β,17β-dihydroxy-16α-methyl-3,20-dioxopregna-1,4-
dien-21-yl
acetate,
D.9-fluoro-11β,17-dihydroxy-16β-methyl-3,20-dioxopregna-1,4-
dien-21-yl acetate(betamethasone acetate),
1810See the information ction on general monographs(cover pages)
EUROPEAN PHARMACOPOEIA 7.0Dexamethasone
isonicotinate
E.9-fluoro-11β,17-dihydroxy-16α-methyl-3,20-dioxopregn-4-en-21-yl
fallout shelter
acetate,
F.17-hydroxy-16α-methyl-3,20-dioxo-9β,11β-epoxypregna-1,4-dien-21-yl
acetate,
G.9-fluoro-11β-hydroxy-16α-methyl-3,20-dioxopregna-1,4-dien-21-yl
acetate,大连教育
H.17-hydroxy-16α-methyl-3,20-dioxopregna-1,4,9(11)-trien-21-yl acetate.
01/2008:2237DEXAMETHASONE ISONICOTINATE Dexamethasoni
isonicotinas C 28H 32FNO 6M r 497.6[2265-64-7]
DEFINITION
9-Fluoro-11β,17-dihydroxy-16α-methyl-3,20-dioxopregna-1,4-dien-21-yl pyridine-4-carboxylate.Content :99.0per cent to 101.0per cent (dried substance).CHARACTERS
Appearance :white or almost white crystalline powder.Solubility :practically insoluble in water,slightly soluble in anhydrous ethanol and in acetone.IDENTIFICATION
Infrared absorption spectrophotometry (2.2.24).Comparison :dexamethasone isonicotinate CRS .
thegraduate
TESTS
Specific optical rotation (2.2.7):+142to +146(dried substance).
Suspend 0.200g in 4.0mL of ethyl acetate R and dilute to 20.0mL with ethanol (96per cent)R .Treat in an ultrasonic bath until a clear solution is obtained.
Related substances .Liquid chromatography (2.2.29).Prepare solutions immediately before u.
Test solution .Suspend 50.0mg in 7mL of acetonitrile R and dilute to 10.0mL with water R .Treat in an ultrasonic bath until a clear solution is obtained.
Reference solution (a).Suspend 5.0mg of dexamethasone CRS and 5.0mg of dexamethasone acetate CRS in 70mL of acetonitrile R ,add 1.0mL of the test solution and dilute to 100.0mL with water R .Treat in an ultrasonic bath until a clear solution is obtained.
Reference solution (b).Dilute 1.0mL of reference solution (a)to 10.0mL with water R .
Reference solution (c).Suspend 5mg of dexamethasone isonicotinate for impurity C identification CRS in 0.7mL of acetonitrile R and dilute to 1mL with water R .Treat in an ultrasonic bath until a clear solution is obtained.Column :
—size :l =0.125m,Ø=4.0mm,
—stationary pha :octadecylsilyl silica gel for chromatography R (5μm).Mobile pha :
—mobile pha A :water R ,
—mobile pha B :acetonitrile R ,
Time (min)Mobile pha A (per cent V/V )
Mobile pha B (per cent V/V )
0-2
68322-2068→5032→5020-2550→6850→3225-35
68
32
Flow rate :1.2mL/min.
toolsDetection :spectrophotometer at 240nm.
Injection :10μL.
Identification of impurities :u the chromatogram
supplied with dexamethasone isonicotinate for impurity C
identification CRS and the chromatogram obtained with reference solution (c)to identify the peak due to impurity C.Relative retention with reference to dexamethasone isonicotinate (retention time =about 12min):impurity A =about 0.4;impurity C =about 0.6;impurity B =about 0.8.
System suitability :reference solution (a):
—resolution :minimum 5.0between the peaks due to
impurity B and dexamethasone isonicotinate.Limits :
相信用英语怎么说—impurity A :not more than 5times the area of the
corresponding peak in the chromatogram obtained with
reference solution (b)(0.5per cent),—impurity B :not more than 3times the area of the
corresponding peak in the chromatogram obtained with
reference solution (b)(0.3per cent),
—impurity C :not more than 3times the area of the peak due to dexamethasone isonicotinate in the chromatogram obtained with reference solution (b)(0.3per cent),
—unspecified impurities :for each impurity,not more than the area of the peak due to dexamethasone isonicotinate in the
chromatogram obtained with reference solution (b)(0.1per
cent),General Notices (1)apply to all monographs and other texts
1811
