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

Itraconazole ni ko kere ju 98.5 ogorun ati pe ko ju 101.5 ogorun ti C35H38Cl2N8O4, ṣe iṣiro lori ipilẹ ti o gbẹ.
Iṣakojọpọ ati ibi ipamọ-Fipamọ sinu wiwọ, awọn apoti sooro ina, ati fipamọ ni iwọn otutu yara.
Awọn ajohunše Itọkasi USP <11>-
USP Itraconazole RS
USP Miconazole RS
Idanimọ-
A: Gbigba infurarẹẹdi <197K>.
Yiyi igun <781A>: laarin -0.10 ° ati + 0.10°, wọn ni 20°
Ojutu idanwo: 100 miligiramu fun milimita, ni methylene kiloraidi
Iwọn yo <741>: laarin 166° ati 170°
Isonu lori gbigbe <731>-Gbẹ nipa 1 g ni 105 ° fun wakati mẹrin: ko padanu ju 0.5% ti iwuwo rẹ.
Aloku lori ina <281>: kii ṣe ju 0.1%, pinnu lori 1.0 g.
Awọn akojọpọ ti o jọmọ-
Solusan A: 0.08 M tetrabutylammonium hydrogen sulfate.
Solusan B: acetonitrile
Diluent-Mura adalu kẹmika ati tetrahydrofuran (1: 1).
Boṣewa ojutu-Tu ohun deede wọn opoiye ti USP Itraconazole RS ni Diluent, stepwise ti o ba wulo y, lati gba a ojutu nini kan mọ ifọkansi ti nipa 0.05 mg fun milimita.
Ojutu ipinnu-Tu awọn iwọn to dara ti USP Itraconazole RS ati USP Miconazole ni RS ni Diluent lati gba ojutu kan ti o ni awọn ifọkansi ti o mọ ti 0.05 miligiramu kọọkan fun milimita kan.
Ojutu idanwo-Tu iwọnwọn Itraconazole ni deede ni Diluent lati gba ojutu kan ti o ni ifọkansi ti a mọ ti bii miligiramu 10 fun miligiramu.
Eto Chromatographic (wo Chromatography <621>) -Kromatograph olomi ti ni ipese pẹlu aṣawari 225-nm ati iwe 4.6-mm × 10-cm ti o ni 3- μm iṣakojọpọ L1.Iwọn sisan jẹ nipa 1.5 milimita fun iṣẹju kan.Iwọn otutu ti ọwọn ti wa ni itọju ni 30 °.Awọn chromatograph ti wa ni siseto bi atẹle
Ojutu akoko A Solusan B
(iṣẹju) (%) (%) Elution
0–20 80→50 20→50 itesiwaju laini
20–25 50 50 isocratic
25-30 80 20 iwontunwonsi
[AKIYESI-Ṣiṣe deede iwe fun o kere ju ọgbọn iṣẹju 30 pẹlu acetonitrile ni iwọn sisan ti 1.5 milimita fun iṣẹju kan ati lẹhinna dọgbadọgba ni akopọ eluent akọkọ fun o kere ju iṣẹju 5.]
Chromatograph ojutu ipinnu, ati ṣe igbasilẹ awọn idahun ti o ga julọ bi a ti ṣe itọsọna fun Ilana: ipinnu, R, laarin miconazole ati itraconazole ko kere ju 2.0.
Ilana-Lọtọ lọ awọn iwọn didun dogba (bii 10 µL) ti Diluent, ojutu Standard ati ojutu idanwo sinu chromatograph ki o ṣe igbasilẹ awọn chromatograms.Ṣe iṣiro ipin ogorun aimọ kọọkan ni apakan Itraconazole ti o mu nipasẹ agbekalẹ:
100(CS/CU)(rU/rS)
ninu eyiti CS jẹ ifọkansi, ni mg fun milimita, ti Itraconazole ni ojutu Standard;CU jẹ ifọkansi, ni miligiramu fun milimita, ti Itraconazole ninu ojutu Idanwo;rU jẹ agbegbe ti o ga julọ fun aimọ kọọkan ninu ojutu Idanwo;ati rS jẹ agbegbe ti o ga julọ fun Itraconazole ni ojutu Standard: kii ṣe ju 0.5% ti eyikeyi aimọ ti a pato, bi a ṣe han ni Table 1, ni a ri;ati pe ko ju 1.25% ti awọn idoti lapapọ ni a rii.Fojusi eyikeyi tente oke ti a ṣe akiyesi ni Diluent ati eyikeyi tente ti o kere ju 0.05%.
Tabili 1
Opin Orukọ Wọpọ (%)
4-Methoxy itọsẹ1 0.5
4-Triazolyl isomer2 0.5
Afọwọṣe propyl3 0.5
isopropyl analog4 0.5
Epimer5 0.5
n-Butyl isomer6 0.5
Didioxolanyl afọwọṣe7 0.5
1 2-aaya-Butyl-4-{4-[4--(4-methoxyphenyl) piperazin-1-yl]phenyl}-2H-1,2,4-triazol-3(4H) -ọkan.
2 4-(4-{4-[4-({(2RS,4SR))-2-[(4H-1,2,4-Triazol-4-yl)methyl]-2-(2,4-dichlorofenyl) -1,3-dioxolan-4-yl}methoxy) phenyl] piperazin-1-yl} phenyl) -2-sec-butyl-2H-1,2,4-triazol-3 (4H) -ọkan.
3 4-(4-{4-[4-({(2RS,4SR))-2-[(1H-1,2,4-Triazol-1-yl)methyl]-2-(2,4-dichlorofenyl) -1,3-dioxolan-4-yl}methoxy) phenyl] piperazin-1-yl} phenyl) -2-propyl-2H-1,2,4-triazol-3 (4H) -ọkan.
4 4-(4-{4-[4-({(2RS,4SR))-2-[(1H-1,2,4-Triazol-1-yl)methyl]-2-(2,4-dichlorofenyl) -1,3-dioxolan-4-yl}methoxy) phenyl] piperazin-1-yl} phenyl) -2-isopropyl-2H-1,2,4-triazol-3 (4H) -ọkan.
5 4- (4-{4-[4-{(2 asoju chelating. 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) -ọkan .
6 4-(4-{4-[4-({(2RS,4SR))-2-[(1H-1,2,4-Triazol-1-yl)methyl]-2-(2,4-dichlorofenyl) -1,3-dioxolan-4-yl}methoxy) phenyl] piperazin-1-yl} phenyl) -2-butyl-2H-1,2,4-triazol-3 (4H) -ọkan.
7 4-(4-{4-[4-({(2RS,4SR))-2-[(1H-1,2,4-Triazol-1-yl)methyl]-2-(2,4-dichlorofenyl) -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) -ọkan.
Ayẹwo-
Diluent-Mura adalu methyl ethyl ketone ati glacial acetic acid (7: 1).
Ilana-tu nipa 0.3 g ti Itraconazole, ni iwọn deede, ni 70 milimita ti Diluent.Titrate pẹlu 0.1 M fun chloric acid, ṣiṣe ipinnu aaye ipari ni agbara ni aaye ifasilẹ keji.milimita kan ti 0.1 M fun chloric acid jẹ deede si 35.3 mg ti C 35H38Cl2N8O4.