all-rac-α-Tocopherol EUROPEAN PHARMACOPOEIA
7.0
Injection :20μL using a refrigerated injector (4-8°C);inject test solution (a)and reference solutions (b),(c)and (d).Run time :1.5times the retention time of tobramycin.Relative retention with reference to tobramycin
(retention time =about 18min):impurity C =about 0.35;impurity B =about 0.40,impurity A =about 0.70.System suitability :
—resolution :minimum 3.0between the peaks due to impurity A and to tobramycin in the chromatogram obtained with reference solution (d);if necessary,adjust the concentration of sodium o
ctanesulfonate in the mobile pha;—signal-to-noi ratio :minimum 10for the principal peak in the chromatogram obtained with reference solution (b).Limits :
—any impurity :not more than twice the area of the principal peak in the chromatogram obtained with reference
solution (c)(1.0per cent)and not more than 1such peak has an area greater than the area of the principal peak in the chromatogram obtained with reference solution (c)(0.5per cent);—total :not more than 3times the area of the principal peak in the chromatogram obtained with reference solution (c)(1.5per cent);
—disregard limit :the area of the principal peak in the
chromatogram obtained with reference solution (b)(0.25per
cent).
2-Methyl-1-propanol (2.4.24,System B ):maximum 1.0per cent m/m .Water (2.5.12):maximum 8.0per cent,determined on 0.30g.Sulfated ash (2.4.14):maximum 0.3per cent,determined on
1.0g.
Bacterial endotoxins (2.6.14):less than 2.0IU/mg,if intended
for u in the manufacture of parenteral preparations without a further appropriate procedure for the removal of bacterial endotoxins.ASSAY
Liquid chromatography (2.2.29)as described in the test for related substances with the following modifications.
Injection :test solution (b)and reference solution (e).
Calculate the percentage content of tobramycin.
STORAGE If the substance is sterile,store in a sterile,airtight,tamper-proof container.
IMPURITIES
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A.4-O -(3-amino-3-deoxy-α-D -glucopyranosyl)-2-deoxy-6-O -(2,6-diamino-2,6-dideoxy-α-D -glucopyranosyl)-L -streptamine (kanamycin
B), B.R =H:2-deoxy-4-O -(2,6-diamino-2,3,6-trideoxy-α-D -ribo-hexopyranosyl)-D -streptamine (nebramine),C.R =OH:2-deoxy-4-O -(2,6-diamino-2,6-dideoxy-α-D -glucopyranosyl)-D -streptamine (
neamine).
01/2008:0692corrected 7.0
all-rac-α-TOCOPHEROL int-rac-α
-Tocopherolum
C 29H 50O 2M r 430.7[10191-41-0]
DEFINITION all-rac -2,5,7,8-Tetramethyl-2-(4,8,12-trimethyltridecyl)-3,4-dihydro-2H -1-benzopyran-6-ol.Content :96.0per cent to 102.0per cent.CHARACTERS
Appearance :clear,colourless or yellowish-brown,viscous,oily liquid.
Solubility :practically insoluble in water,freely soluble in acetone,in anhydrous ethanol,in methylene chloride and in fatty oils.
IDENTIFICATION
First identification:A,B.
Second identification:A,C.
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A.Optical rotation (2.2.7):−0.01°to +0.01°.
Dissolve 2.50g in anhydrous ethanol R and dilute to
25.0mL with the same solvent.
人人听力B.Infrared absorption spectrophotometry (2.2.24).Comparison :α-tocopherol CRS .
C.Thin-layer chromatography (2.2.27).
Test solution .Dissolve 10mg of the substance to be examined in 2mL of cyclohexane R .
Reference solution.Dissolve 10mg of α-tocopherol CRS in 2mL of cyclohexane R .
Plate :TLC silica gel F 254plate R .
Mobile pha :ether R ,cyclohexane R (20:80V/V ).Application :10μL.
Development :over 2/3of the plate.Drying :in a current of 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 principal spot in the chromatogram obtained with the reference solution.3104
See the information ction on general monographs (cover pages)
EUROPEAN PHARMACOPOEIA 7.0RRR -α别对我撒谎第一季
-Tocopherol
TESTS
Related substances .Gas chromatography (2.2.28):u the normalisation procedure.
Internal standard solution .Dissolve 1.0g of squalane R in cyclohexane R and dilute to 100.0mL with the same solvent.Test solution (a).Dissolve 0.100g of the substance to be examined in 10.0mL of the internal standard solution.Test solution (b).Dissolve 0.100g of the substance to be examined in 10mL of cyclohexane R .
Reference solution (a).Dissolve 0.100g of α-tocopherol CRS in 10.0mL of the internal standard solution.
Reference solution (b).Dissolve 10mg of the substance to be examined and 10mg of α-tocopheryl acetate R in
cyclohexane R and dilute to 100.0mL with the same solvent.Reference solution (c).Dissolve 10mg of all-rac-α-tocopherol for peak identification CRS (containing impurities A and B)in cyclohexane R and dilute to 1mL with the same solvent.Reference solution (d).Dilute 1.0mL of test solution (b)to 100.0mL with cyclohexane R .Dilute 1.0mL of this solution to 10.0mL with cyclohexane R .Column :
—material :fud silica;
—size :l =30m,Ø=0.25mm;
—stationary pha :poly(dimethyl)siloxane R (film thickness 0.25μm).
Carrier gas :helium for chromatography R .Flow rate :1mL/min.Split ratio :1:100.Temperature :
—column :280°C;
—injection port and detector :290°C.Detection :flame ionisation.
Injection :1μL of test solution (b)and reference solutions (b),(c)and (d).
Run time :twice the retention time of all-rac -α-tocopherol.Identification of impurities :u the chromatogram supplied with all-rac-α-tocopherol for peak identification CRS and the chromatogram obtained with reference solution (c)to identify the peaks due to impurities A and B.
Relative retention with reference to all-rac -α-tocopherol (retention time =about 13min):squalane =about 0.5;larger
impurity A =about 0.7;impurity B =about 0.8;impurities C and D =about 1.05(eluting immediately after the all-rac -α-tocopherol peak).
System suitability :reference solution (b):
—resolution :minimum 3.5between the peaks due to all-rac -α-tocopherol and α-tocopheryl acetate.Limits :
bigbreast—impurity A :maximum 0.5per cent;—impurity B :maximum 1.5per cent;
—sum of impurities C and D :maximum 1.0per cent;
tci—any other impurity :for each impurity,maximum 0.25per cent;
omt
—total :maximum 2.5per cent;
—disregard limit :the area of the principal peak in the
chromatogram obtained with reference solution (d)(0.1per cent).
The thresholds indicated under Related substances
(Table 2034.-1)in the general monograph Substances for pharmaceutical u (2034)do not apply.
ASSAY
Gas chromatography (2.2.28)as described in the test for related substances with the following modification.
Injection :test solution (a)and reference solution (a).
Calculate the percentage content of C 29H 50O 2from the declared content of α-tocopherol CRS .
STORAGE
Under an inert gas,protected from light.IMPURITIES
Specified impurities:A,B,C,D
.
A.all-rac -trans -2,3,4,6,7-pentamethyl-2-(4,8,12-
trimethyltridecyl)-2,3-dihydrobenzofuran-5-ol,
B.all-rac -cis -2,3,4,6,7-pentamethyl-2-(4,8,12-trimethyltridecyl)-
2,3-dihydrobenzofuran-5-ol.
C.4-methoxy-2,3,6-trimethyl-5-[(all-RS ,E )-3,7,11,15-
tetramethylhexadec-2-enyl]phenol,
D.(all-RS ,all-E )-2,6,10,14,19,23,27,31-octamethyldotriaconta-12,14,18-triene.
01/2008:1256
RRR -α-TOCOPHEROL RRR -α
storage是什么意思
-Tocopherolum
C 29H 50O 2M r 430.7
[59-02-9]
DEFINITION
(2R )-2,5,7,8-Tetramethyl-2-[(4R ,8R )-4,8,12-trimethyltridecyl]-3,4-dihydro-2H -1-benzopyran-6-ol.
potential是什么意思Content :94.5per cent to 102.0per cent.
General Notices (1)apply to all monographs and other texts
3105
