Tom ntej: Itraconazole CAS 84625-61-6 Assay 98.5 ~ 101.5%

Itraconazole muaj tsis tsawg tshaj li 98.5 feem pua ​​thiab tsis ntau tshaj 101.5 feem pua ​​ntawm C35H38Cl2N8O4, xam nyob rau hauv qhuav.
Ntim thiab khaws cia-Txuag hauv cov thawv nruj, lub teeb-tiv taus, thiab khaws cia ntawm chav tsev kub.
USP Reference cov qauv <11>-
USP Itraconazole RS
USP Miconazole RS
Kev txheeb xyuas-
A: Infrared Absorption <197K>.
Angular rotation <781A>: ntawm -0.10 ° thiab + 0.10 °, ntsuas ntawm 20 °
Test tov: 100 mg ib mL, nyob rau hauv methylene chloride
Melting ntau <741>: ntawm 166 ° thiab 170 °
Poob ntawm ziab <731>-Sry txog 1 g ntawm 105 ° rau 4 teev: nws poob tsis ntau tshaj 0.5% ntawm nws qhov hnyav.
Residue ntawm ignition <281>: tsis ntau tshaj 0.1%, txiav txim siab ntawm 1.0 g.
Related compounds-
Tshuaj A: 0.08 M tetrabutylammonium hydrogen sulfate.
Kev daws B: acetonitrile
Diluent-Npaj sib tov ntawm methanol thiab tetrahydrofuran (1: 1).
Cov txheej txheem kev daws teeb meem-Dissolve ib qhov hnyav hnyav ntawm USP Itraconazole RS hauv Diluent, stepwise yog tias tsim nyog y, kom tau txais ib qho kev daws teeb meem uas paub txog ntawm 0.05 mg ib mL.
Kev daws teeb meem-Dissolve tsim nyog kom muaj nuj nqis ntawm USP Itraconazole RS thiab USP Miconazole hauv RS hauv Diluent kom tau txais cov tshuaj uas muaj kev paub txog ntau npaum li 0.05 mg txhua ib mL.
Test solution-Dissolve ib qho hnyav hnyav ntawm Itraconazole hauv Diluent kom tau txais kev daws teeb meem uas paub txog qhov concentration ntawm li 10 mg ib mL.
Chromatographic system (saib Chromatography <621>)-Cov kua chromatograph yog nruab nrog 225-nm detector thiab 4.6-mm × 10-cm kem uas muaj 3- μm packing L1.Tus nqi ntws yog li 1.5 mL ib feeb.Qhov kub thiab txias yog khaws cia ntawm 30 °.Lub chromatograph yog programmed raws li nram no
Lub Sijhawm Kev daws A Kev daws B
(feeb) (%) (%) Elution
0-20 80 → 50 20 → 50 linear gradient
20–25 50 50 IB
25-30 80 20 equilibration
[CEEB TOOM-Equilibrate kem rau yam tsawg kawg 30 feeb nrog acetonitrile ntawm ib tug txaus tus nqi ntawm 1.5 mL ib feeb thiab ces sib npaug ntawm thawj eluent muaj pes tsawg leeg rau tsawg kawg yog 5 feeb.]
Chromatograph qhov kev daws teeb meem, thiab sau cov lus teb siab tshaj plaws raws li qhia rau Kev Ua Haujlwm: kev daws teeb meem, R, nruab nrab ntawm miconazole thiab itraconazole tsis tsawg dua 2.0.
Cov txheej txheem-Kev txhaj tshuaj sib npaug sib npaug (kwv yees li 10 µL) ntawm Diluent, Standard tov thiab Test tov rau hauv chromatograph thiab sau cov chromatograms.Xam cov feem pua ​​​​ntawm txhua qhov impurity hauv ib feem ntawm Itraconazole coj los ntawm cov mis:
100 (CS / CU) (rU / rS)
nyob rau hauv uas CS yog qhov concentration, hauv mg ib mL, ntawm Itraconazole hauv Standard tov;CU yog qhov concentration, nyob rau hauv mg ib mL, ntawm Itraconazole nyob rau hauv cov tshuaj ntsuam xyuas;rU yog qhov chaw siab tshaj plaws rau txhua qhov impurity hauv Kev Ntsuas Kev Ntsuas;thiab rS yog qhov chaw siab tshaj plaws rau Itraconazole hauv cov txheej txheem kev daws teeb meem: tsis pub ntau tshaj 0.5% ntawm cov impurity uas tau teev tseg, raws li qhia hauv Table 1, pom;thiab tsis pub ntau tshaj 1.25% ntawm tag nrho cov impurities pom.Tsis quav ntsej txhua qhov ncov pom hauv Diluent thiab ib qho ncov tsawg dua 0.05%.
Table 1
Hom Lub Npe Limit (%)
4-Methoxy derivative 1 0.5
4-Triazolyl isomer2 0.5
Propyl analog3 0.5
Isopropyl analogue 4 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)-ib.
2 4-(4-{4-[4-(((2RS,4SR))-2-[(4H-1,2,4-Triazol-4-yl)methyl]-2,4-dichlorophenyl)) -1,3-dioxolan-4-yl}methoxy)phenyl]piperazin-1-yl}phenyl)-2-sec-butyl-2H-1,2,4-triazol-3(4H)-ib.
3 4-(4-{4-[4-((2RS,4SR)-2-[(1H-1,2,4-Triazol-1-yl)methyl]-2,4-dichlorophenyl)) -1,3-dioxolan-4-yl}methoxy)phenyl]piperazin-1-yl}phenyl)-2-propyl-2H-1,2,4-triazol-3(4H)-ib.
4 4-(4-{4-[4-(((2RS,4SR))-2-[(1H-1,2,4-Triazol-1-yl)methyl]-2,4-dichlorophenyl)) -1,3-dioxolan-4-yl}methoxy)phenyl]piperazin-1-yl}phenyl)-2-isopropyl-2H-1,2,4-triazol-3(4H)-ib.
5 4-(4-{4-[4-({(2 chelate agents. 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)-ib .
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)-ib.
7 4-(4-{4-[4-(((2RS,4SR))-2-[(1H-1,2,4-Triazol-1-yl)methyl]-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)-ib.
Assay-
Diluent-Npaj sib tov ntawm methyl ethyl ketone thiab glacial acetic acid (7: 1).
Cov txheej txheem - Dissolve txog 0.3 g ntawm Itraconazole, raug hnyav, hauv 70 ml ntawm Diluent.Titrate nrog 0.1 M ib chloric acid, txiav txim siab qhov kawg potentiometrically ntawm qhov thib ob inflection point.Ib mL ntawm 0.1 M ib chloric acid yog sib npaug rau 35.3 mg ntawm C 35H38Cl2N8O4.