Itraconazole CAS 84625-61-6 Intende 98.5~ 101.5%

Itraconazolum non minus quam 98.5 centesimas continet et non plus quam 101.5 centesimas C35H38Cl2N8O4, in fundamento aridae computatum.
Packaging ac repono-Conserve in angustiis, vasis levibus repugnantibus, et ad cella temperiei repone.
USP Reference signa <11>-
USP Itraconazole RS
USP Miconazole RS
Identification-
A: Absorptio infrared <197K>.
Rotatio angularis <781A>: inter -0.10° et +0.10°, mensurata 20°
Solutio test: 100 mg per mL, in chloride methylene
Distinctio range <741>: inter 166° et 170° .
Damnum in siccitate <731>-Arida circa 1 g ad 105° pro 4 horis: non plus quam 0.5% sui ponderis amittit.
Residere ignitionem <281>: non plus quam 0.1%, constituta in 1.0 g.
Related compounds-
Solutio A: 0.08 M hydrogenium tetrabutylammonium sulfate.
Solutio B: acetonitrile
Diluent-Para mixturam methanoli et tetrahydrofurani (1:1).
Solutio Standard - Disolve quantitatem Itraconazoli RS in Diluent, gradatim si necesse est y accurate ponderatam quantitatem USP, solutionem habere notam circa 0,05 mg per mL.
Resolutio solutionis solvendi quantitates idoneas USP Itraconazoli RS et USP Miconazoli in RS in Diluent ad solutionem obtinendam cum notis concentratione circiter 0,05 mg singulorum per mL.
Solutio test-dissolve quantitatem Itraconazoli accurate ponderatam in Diluent ad solutionem obtinendam habens notam intentionem circiter 10 mg per mL.
Systema chromatographicum (cf. chromatographia <621>) - chromatographum liquidum cum detectore 225-um et 4.6-mm × 10-cm instructum est columna quae continet 3- μm fasciculum L1.Rate fluxus circiter 1.5 mL per minute est.Columpna temperatura 30° conservata est.Chromatographum programmatum est ut sequitur
Tempus Solutio B
(minuta) (%) (%) Elution
0-20 80 → 50 20 → 50 linearium clivum
20-25 50 50 isocraticus
25-30 80 20 aequilibratio
[Nota-aequilibrare columnam ad minimum 30 minuta cum acetonitrili ad ratem fluxum 1.5 mL per minutum, et tunc aequilibratum in compositione initiali eluenti pro 5 minuta saltem.
Solutio chromatographa resolutio, et refero apicem responsionum ad procedendum directae: resolutio R, inter miconazolum et itraconazolum non minus quam 2.0.
De modo procedendi-Separatim inferunt paria volumina (circa 10 µL) de diluente, solutione vexillifer et solutione test in chromatographa et chromatogrammata notant.Recipis cujusvis immunditiae in portione Itraconazoli sumpta formula;
100(CS/CU)(rU/rS)
in quo CS est concentratio in mg per mL, Itraconazoli in solutione Vexillima;CU est intentio, in mg per mL, Itraconazoli in solutione test;rU area ad cujuslibet immunditiae apicem in teftium solutione ;and rS is the cacumen area for Itraconazole in the Standard solution: not more than 0.5% of any specified impurity, as shown in Table 1, is found;et non plus quam 1.25% totius immunditiae invenimus.Nullum apicem observatum in Diluent et in quolibet cacumine minus quam 0.05% negligere.
Table 1
Communi nomine Limit (%)
4-Methoxy derivativum1 0.5
4-Triazolyl isomer2 0.5
Propyl analog3 0.5
Isopropyl analog4 0.5
Epimer5 0.5
n-Butyl isomer6 0.5
Didioxolanyl analog7 0.5
1 2-sec-Butyl-4-{4-[4-(4-methoxyphenyl)piperazin-1-yl]phenyl}-2H-1,2,4-triazol-3(4H)-one.
2 4-(4-{4-[4-({(2RS,4SR)-2-[(4H-1,2,4-Triazol-4-yl)methyl]-2-(2,4-dichlorophenyl) -1,3-dioxolan-4-yl}methoxy)phenyl]piperazin-1-yl}phenyl)-2-sec-butyl-2H-1,2,4-triazol-3(4H)-one.
3 4-(4-{4-[4-({(2RS,4SR)-2-[(1H-1,2,4-Triazol-1-yl) methyl]-2-(2,4-dichlorophenyl) -1,3-dioxolan-4-yl}methoxy)phenyl]piperazin-1-yl}phenyl)-2-propyl-2H-1,2,4-triazol-3(4H)-one.
4 4-(4-{4-[4-({(2RS,4SR)-2-[(1H-1,2,4-Triazol-1-yl) methyl]-2-(2,4-dichlorophenyl) -1,3-dioxolan-4-yl}methoxy)phenyl]piperazin-1-yl}phenyl)-2-isopropyl-2H-1,2,4-triazol-3(4H)-one.
5 4-(4-{4-[4-({(2 agentium fraudantes. RS,4RS)-2-[(1H-1,2,4-Triazol-1-yl)methyl]-2-(2; 4-dichlorophenyl)-1,3-dioxolan-4-yl}methoxy)phenyl]piperazin-1-yl}phenyl)-2-sec-butyl-2H-1,2,4-triazol-3(4H)-one .
6 4-(4-{4-[4-({(2RS,4SR)-2-[(1H-1,2,4-Triazol-1-yl) methyl]-2-(2,4-dichlorophenyl) -1,3-dioxolan-4-yl}methoxy)phenyl]piperazin-1-yl}phenyl)-2-butyl-2H-1,2,4-triazol-3(4H)-one.
7 4-(4-{4-[4-({(2RS,4SR)-2-[(1H-1,2,4-Triazol-1-yl) methyl]-2-(2,4-dichlorophenyl) -1,3-dioxolan-4-yl}methoxy)phenyl]piperazin-1-yl}phenyl)-2-({(2RS,4SR)-2-[(1H-1,2,4-triazol-1- yl)methyl]-2-(2,4-dichlorophenyl)-1,3-dioxo-lan-4-yl}methyl)-2H-1,2,4-triazol-3(4H)-one.
Assay-
Diluente-Para mixturam metri ethyl ketonis et glacialis acetici (7, 1).
Procedure-Dissolve circa 0,3 g Itraconazole accurate perpensa, in 70 ml Diluent.Titrate cum 0.1 M per acidum chloricum, terminum potentiometrice determinans ad punctum secundae declinationis.Una mL acidi per chlorici 0.1 M aequivalet 35.3 mg C 35H38Cl2N8O4.