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Propofol丙泊酚 silica gel正相柱  

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 Propofol丙泊酚 silica gel正相柱

British Pharmacopoeia 2009
British Pharmacopoeia Volume I & II
Monographs: Medicinal and Pharmaceutical Substances
Propofol
Propofol
General Notices
(Ph Eur monograph 1558)
C12H18O??178.3??2078-54-8
Action and use
Intravenous general anaesthetic.
Preparation
Propofol Injection
Ph Eur
DEFINITION
2,6-Bis(1-methylethyl)phenol.
Content
98.0 per cent to 102.0 per cent.
This monograph applies to propofol prepared using distillation for purification.
CHARACTERS
Appearance
Colourless or very light yellow, clear liquid.
Solubility
Very slightly soluble in water, miscible with hexane and with methanol.
IDENTIFICATION
Infrared absorption spectrophotometry (2.2.24).
Comparison?propofol CRS.
TESTS
Refractive index (2.2.6): 1.5125 to 1.5145.
Related substances
Liquid chromatography (2.2.29).
Test solution (a)?Dissolve 1.00 g of the substance to be examined in hexane R and dilute to
10.0 ml with the same solvent.
Test solution (b)?Dissolve 0.240 g of the substance to be examined in hexane R and dilute to
100.0 ml with the same solvent.
Reference solution (a)?Dissolve 5 μl of the substance to be examined and 15 μl of propofol
impurity J CRS in hexane R and dilute to 50.0 ml with the same solvent.
Reference solution (b)?Dilute 0.1 ml of propofol for peak identification CRS (containing
impurities E and G) to 1.0 ml with hexane R.
Reference solution (c)?Dilute 1.0 ml of test solution (a) to 100.0 ml with hexane R. Dilute 1.0
ml of this solution to 10.0 ml with hexane R.
Reference solution (d)?Dissolve 0.240 g of propofol CRS in hexane R and dilute to 100.0 ml
with the same solvent.
Column: ?
?— size: l = 0.20 m, ? = 4.6 mm;
?— stationary phase: silica gel for chromatography R (5 μm).
Mobile phase?anhydrous ethanol R, acetonitrile R, hexane R (1.0:7.5:990 V/V/V).
Flow rate?2.0 ml/min.
Detection? Spectrophotometer at 275 nm.
Injection?10 μl of test solution (a) and reference solutions (a), (b) and (c).
Run time?7 times the retention time of propofol.
Identification of impurities?Use the chromatogram obtained with reference solution (b) to
identify the peaks due to impurities G and E.
Relative retention?With reference to propofol (retention time = about 3 min): impurity G =
about 0.5; impurity I = about 0.6; impurity B = about 0.7; impurity N = about 2.3; impurity D =
about 2.5; impurity P = about 2.9; impurity A = about 3.0; impurity C = about 3.4; impurity E =
about 4.0; impurity F = about 5.8; impurity H = about 6.4.
System suitability? Reference solution (a):
?— resolution: minimum 4.0 between the peaks due to impurity J and propofol.
Limits:
?— correction factors: for the calculation of content, multiply the peak areas of the following
impurities by the corresponding correction factor: impurity E = 0.25; impurity G = 5.0;
?— impurity G: not more than twice the area of the peak due to propofol in the chromatogram
obtained with reference solution (c) (0.2 per cent);
?— impurity E: not more than 0.1 times the area of the peak due to propofol in the
chromatogram obtained with reference solution (c) (0.01 per cent);
?— unspecified impurities: for each impurity, not more than 0.5 times the area of the peak
?— unspecified impurities: for each impurity, not more than 0.5 times the area of the peak
due to propofol in the chromatogram obtained with reference solution (c) (0.05 per cent);
?— total: not more than 3 times the area of the peak due to propofol in the chromatogram
obtained with reference solution (c) (0.3 per cent);
?— disregard limit: 0.3 times the area of the peak due to propofol in the chromatogram
obtained with reference solution (c) (0.03 per cent), except for impurity E.
Impurities J, K, L and O
Gas chromatography (2.2.28).
Test solution?Dissolve 40.0 mg of the substance to be examined in methylene chloride R and
dilute to 10.0 ml with the same solvent.
Reference solution (a)?Dilute 1.0 ml of the test solution to 100.0 ml with methylene chloride
R. Dilute 1.0 ml of this solution to 10.0 ml with methylene chloride R.
Reference solution (b)?Dissolve 5 μl of propofol impurity J CRS (corresponding to 5 mg) in
methylene chloride R and dilute to 100 ml with the same solvent. Dilute 1.0 ml of this solution
to 25 ml with methylene chloride R.
Reference solution (c)?Dissolve 4 mg of propofol CRS in reference solution (b) and dilute to 1
ml with the same solution.
Column: ?
?— material: fused silica;
?— size: l = 30 m, ? = 0.32 mm;
?— stationary phase: polymethylphenylsiloxane R (film thickness 0.5 μm).
Carrier gas?helium for chromatography R.
Flow rate?1.7 ml/min.
Split ratio?1:5.
Temperature:
Detection?Flame ionisation.
Injection?1 μl of the test solution and reference solutions (a) and (c).
Relative retention?With reference to propofol (retention time = about 17 min): impurity K =
about 0.76; impurity L = about 0.81; impurity J = about 1.01; impurity O = about 1.03.
System suitability?Reference solution (c):
System suitability?Reference solution (c):
?— peak-to-valley ratio: minimum 3.0, where Hp = height above the baseline of the peak due
to impurity J, and Hv = height above the baseline of the lowest point of the curve separating
this peak from the peak due to propofol.
Limits:
?— impurities J, K, L, O: for each impurity, not more than 0.5 times the area of the principal
peak in the chromatogram obtained with reference solution (a) (0.05 per cent).

Liquid chromatography (2.2.29) as described in the test for related substances with the
following modification.
Injection?Test solution (b) and reference solution (d).
Calculate the percentage content of C12H18O using the declared content of propofol CRS.
STORAGE
Protected from light under an inert gas.
IMPURITIES
Specified impurities?E, G, J, K, L, O.
Other detectable impurities?(The following substances would, if present 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 use (2034). It is therefore not necessary to identify these
impurities for demonstration of compliance. See also 5.10. Control of impurities in substances
for pharmaceutical use): A, B, C, D, F, H, I, N, P.
?A. R1 = CH(CH3)2, R2 = R3 = H: 2,4-bis(1-methylethyl)phenol,
?B. R1 = R2 = H, R3 = C(CH3)=CH2: 2-(1-methylethenyl)-6-(1-methylethyl)phenol,
?C. R1 = R2 = R3 = H: 2-(1-methylethyl)phenol,
?D. R1 = R3 = H, R2 = CH(CH3)2: 2,5-bis(1-methylethyl)phenol,
?N. R1 = CO2H, R2 = H, R3 = CH(CH3)2: 4-hydroxy-3,5-bis(1-methylethyl)benzoic acid,
?O. R1 = R2 = H, R3 = CH2-CH2-CH3: 2-(1-methylethyl)-6-propylphenol,
?P. R1 = CO-O-CH(CH3)2, R2 = H, R3 = CH(CH3)2: 1-methylethyl 4-hydroxy-3,5-bis(1-
methylethyl)benzoate,
?E. 3,3?,5,5?-tetrakis(1-methylethyl)biphenyl-4,4?-diol,
?F. R = CH(CH3)2, R? = H: 3-(1-methylethyl)phenol,
?H. R = H, R? = CH(CH3)2: 4-(1-methylethyl)phenol,
?G. R = CH(CH3)2: 2-(1-methylethoxy)-1,3-bis(1-methylethyl)benzene,
?K. R = H: 1-(1-methylethoxy)-2-(1-methylethyl)benzene,
?I. oxydibenzene,
?J. 2,6-bis(1-methylethyl)benzene-1,4-dione,
?L. 2,2-dimethyl-4-(1-methylethyl)-1,3-benzodioxole.

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