EUROPEAN PHARMACOPOEIA 6.0
Imipenem IMPURITIES Specified impurities :A,B,C,E,F.Other detectable impurities:D.Related
considerablysubstances test A
meritocracy
A.3-[(2-chloroethyl)amino]propyl dihydrogen phosphate,
B.
xiangfan
bis[3-[(2-chloroethyl)amino]propyl]dihydrogen diphosphate,C.R =Cl:2-chloroethanamine,D.R =OH:2-aminoethanol.
Related substances test B
E.3-chloro-N -(2-chloroethyl)propan-1-amine,
F.(RS )-2-chloro-3-(2-chloroethyl)-1,3,2-oxazaphosphinane 2-oxide.01/2008:1226
corrected 6.0IMIPENEM Imipenemum C 12H 17N 3O 4S,H 2O M r 317.4DEFINITION (5R ,6S )-6-[(R )-1-Hydroxyethyl]-3-[[2-[(iminomethyl)amino]-
ethyl]sulphanyl]-7-oxo-1-azabicyclo[3.2.0]hept-2-ene-2-carboxylic acid monohydrate.Semi-synthetic product derived from a fermentation product.
Content :98.0per cent to 102.0per cent (anhydrous substance).CHARACTERS Appearance :white or
almost white or pale yellow powder.
日语新年快乐怎么说Solubility :sparingly soluble in water,slightly soluble in methanol.IDENTIFICATION
Infrared absorption spectrophotometry (2.2.24).Comparison :imipenem CRS .
TESTS
Appearance of solution .The solution is not more opalescent
than reference suspension II (2.2.1)and not more intenly
coloured than intensity 6of the range of the reference solutions of the most appropriate colour (2.2.2,Method II ).
Dissolve 0.500g in phosphate buffer solution pH 7.0R3and
dilute to 50ml with the same solution.pH (2.2.3):4.5to 7.0.
Dissolve 0.500g in carbon dioxide-free water R and dilute
to 100.0ml with the same solvent.Specific
optical rotation (2.2.7):+84to +89(anhydrous
substance),measured at 25°C.Dissolve 0.125g in phosphate buffer solution pH 7.0R3and
dilute to 25.0ml with the same solution.Related
substances .Liquid chromatography
(2.2.29).Keep the solutions in an ice-bath and u within 8h of preparation.Solvent mixture .Mix 0.7volumes of acetonitrile R and
challengeable
99.3volumes of a 0.135g/l solution of dipotassium
hydrogen phosphate R adjusted to pH 6.8with dilute
phosphoric acid R .Test solution .Dissolve 40.0mg
of the substance to be examined in the solvent mixture and dilute to 100.0ml with
the solvent mixture.Reference solution (a).Dissolve 40.0mg of imipenem CRS
in the solvent mixture and dilute to 100.0ml with the solvent mixture.Reference
solution (b).Dilute 1.0ml of the test solution to
100.0ml with the solvent mixture.Reference solution (c).Heat 20ml of the test solution,
previously adjusted to pH 10with sodium hydroxide solution
R ,at 80°C for 5min (in situ preparation of
impurity A).Column :
—size :l =0.25m,Ø=4.6mm;
—stationary pha :octadecylsilyl silica gel for
chromatography R (5µm).Mobile pha :mix 0.7volumes of acetonitrile
R and
99.3volumes
of a 8.7g/l solution of dipotassium hydrogen
phosphate R adjusted to pH 7.3with dilute phosphoric acid R .Flow rate :1.0ml/min.
Detection :spectrophotometer at 254nm.Injection
:20µl of the test solution and reference solutions (b)and (c).Run time :twice the retention time of imipenem.Relative retention with reference to imipenem (retention time =about 9min):impurity A =about 0.8.System suitability :reference solution (c):
—resolution :minimum 3.5between the peaks due to impurity A and imipenem.Limits :
—impurity
A :not more than the area of
the principal peak in the chromatogram obtained with reference solution (b)
(1per cent);General Notices (1)apply to all monographs and other texts 2125
Imipramine hydrochloride EUROPEAN PHARMACOPOEIA
6.0—any other impurity :for each impurity,not more than 0.3times the area of the principal peak in th
e chromatogram obtained with reference solution (b)(0.3per cent);—sum of impurities other than A :not more than the area
of the principal peak in the chromatogram obtained with reference solution (b)(1per cent);—disregard limit :0.1times the area of the principal peak in the chromatogram obtained with reference solution (b)(0.1per cent).Water (2.5.12):5.0per cent to 8.0per cent,determined
on 0.200g.U an iodosulphurous reagent containing imidazole instead of pyridine and a clean container for each determination.Sulphated ash (2.4.14):maximum 0.2per cent,determined
on 1.0g.Bacterial endotoxins (2.6.14):less than 0.17IU/mg,if intended for u
祈使句的回答
in the manufacture of parenteral dosage forms without a further appropriate procedure for 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 and reference solution (a).System suitability :reference solution (a):—repeatability :maximum relative standard deviation of 1.0per cent after 6injections.STORAGE In an airtight container,
at a temperature of 2°C to
8°C.If the substance is sterile,store in a sterile,airtight,tamper-proof container.IMPURITIES Specified impurities :
A.A.(5R ,6S )-3-[(2-aminoethyl)sulphanyl]-6-[(R )-1-hydroxyethyl]-7-oxo-1-azabicyclo[3.2.0]hept-2-ene-2-carboxylic acid (thienamycin).01/2008:0029corrected 6.0IMIPRAMINE HYDROCHLORIDE Imipramini
hydrochloridum C 19H 25ClN 2M r 316.9[113-52-0]DEFINITION
Imipramine
复习计划hydrochloride contains not less than 98.5per cent
and not more than the equivalent of 101.0per cent of 3-(10,11-dihydro-5H -dibenzo[b,f ]azepin-5-yl)-N ,N -dimethylpropan-1-amine hydrochloride,calculated with
reference to the dried substance.CHARACTERS
A
white or slightly yellow,crystalline powder,freely soluble in water and in alcohol.IDENTIFICATION
First identification:A,C,F.
Second identification:A,B,D,E,F.
A.Melting point (2.2.14):170°C to 174°C.
B.Dissolve
20mg in 0.01M hydrochloric acid and dilute to 100.0
ml with the same acid.Dilute 1.0ml of the solution
to 10.0ml
with 0.01M hydrochloric acid .Examined
between 230nm and 350nm,the solution shows a single
absorption maximum (2.2.25),at 251nm,and a shoulder at 270nm.The specific absorbance at the maximum is
about 260.C.Examine by infrared absorption spectrophotometry (
2.2.24),comparing with the spectrum obtained with imipramine hydrochloride CRS .Examine the substances prepared as discs.D.Dissolve
about 5mg in 2ml of nitric acid R .An inten blue colour develops.E.Dissolve about 50mg in 3ml
of water R and add 0.05ml
of a 25g/l solution of quinhydrone R in methanol R .No
red colour develops within 15min.F.About 20mg gives reaction (a)of chlorides (2.3.1).
TESTS
Solution S .To 3.0g add 20ml of carbon dioxide-free
water R ,dissolve rapidly by shaking and triturating with a
glass rod and dilute to 30ml with the same solvent.Appearance of solution .
英文动画片Solution
S is clear (2.2.1).
Immediately after
preparation,dilute solution S with an
equal volume of water R .This solution is not more intenly coloured than reference solution BY 6(2.2.2,Method II ).
pH (2.2.3).The pH of solution S,measured immediately after preparation,is 3.6to 5.0.
Related substances .Examine by thin-layer chromatography
(2.2.27),using a TLC silica gel G plate R .Test
solution.Dissolve 0.25g of the substance to be examined in methanol R and dilute to 10ml with the same
solvent.Prepare immediately before u.
Reference
solution (a).Dilute 1ml of the test solution to
10ml with methanol R .Dilute 1ml of this solution to 50ml
with methanol R .Reference solution (b).Dissolve 5mg
rollingof iminodibenzyl R
in methanol R and dilute to 100ml with the same solvent.Prepare immediately before u.Apply to the plate
10µl of each solution.Develop over a信息学
path of 12cm using a mixture of 5volumes of hydrochloric
acid R ,5volumes of water R ,35volumes of glacial acetic acid R and 55volumes of ethyl acetate R .Allow the plate
to dry in air for
5min and spray with a 5g/l solution
of potassium dichromate R in a mixture of 1volume of
sulphuric acid R and 4volumes of water R .Examine the plate immediately.The chromatogram obtained with the test solution shows a blue principal spot.In the chromatogram obtained with the test solution:any spot corresponding 2126See the information ction on general monographs (cover pages)
