Gemcitabine Hydrochloride CAS 122111-03-9 API USP35 Tus Qauv

Gemcitabine Hydrochloride
C9H11F2N3O4 · HCl 299.66
Cytidine, 2'-deoxy-2', 2'-difluro-, monohydrochloride.
2′-Deoxy-2′,2′-difluorocytidine monohydrochloride (β-isomer) [122111-03-9].
» Gemcitabine Hydrochloride muaj tsis pub tsawg dua 97.5 feem pua ​​thiab tsis ntau tshaj 101.5 feem pua ​​ntawm C9H11F2N3O4·HCl, xam raws li lub hauv paus.
[Ceev faj-Gemcitabine Hydrochloride yog ib tug muaj zog cytotoxic tus neeg sawv cev.Kev saib xyuas zoo yuav tsum tau coj los tiv thaiv kom tsis txhob nqus cov khoom thiab nthuav tawm ntawm daim tawv nqaij rau nws.]
Ntim thiab khaws cia-Txuag hauv cov thawv nruj.
Labeling-Qhov twg nws yog npaj los siv rau hauv kev npaj cov tshuaj txhaj tshuaj, daim ntawv lo hais tias nws tsis muaj menyuam lossis yuav tsum tau ua ntxiv thaum lub sijhawm npaj cov ntawv txhaj tshuaj.
USP Reference cov qauv <11>-
USP Cytosine RS
Tom ntej: USP Endotoxin RS
USP Gemcitabine Hydrochloride RS
Kev txheeb xyuas-
A: Infrared Absorption <197K>.
B: Nws ua tau raws li qhov yuav tsum tau ua ntawm kev sim rau Chloride <191>.
Kev sib hloov tshwj xeeb <781S>: nruab nrab ntawm +43 thiab +50, ntawm 20.
Test tov: 10 mg ib mL.
pH <791>: nruab nrab ntawm 2.0 thiab 3.0, hauv cov tshuaj muaj 10 mg ib mL.
Residue ntawm ignition <281>: tsis ntau tshaj 0.1%.
Cov hlau hnyav, Txoj Kev I <231>: 0.001%.
Chromatographic purity-
Kev daws A- Ua tiav raws li tau hais tseg rau theem Mobile hauv Kev Tshawb Fawb.
Tshuaj B-Npaj lim thiab degassed methanol.
Txawb theem-Siv sib txawv ntawm cov tshuaj A thiab tshuaj B raws li qhia hauv Chromatographic system.Ua kev hloov kho, yog tias tsim nyog (saib System Suitability hauv Chromatography 621).
System suitability solution-Ua raws li qhia hauv Assay.
Cov txheej txheem kev daws teeb meem-Dissolve kom raug qhov hnyav ntawm USP Gemcitabine Hydrochloride RS thiab USP Cytosine RS hauv dej, thiab dilute quantitatively, thiab stepwise yog tias tsim nyog, kom tau txais cov kev daws teeb meem uas paub txog txog 2 µg ib mL ntawm txhua.
Kev ntsuas tshuaj-Hloov li 50 mg ntawm Gemcitabine Hydrochloride, ntsuas kom raug, mus rau 25-mL ntim ntim, yaj hauv thiab dilute nrog dej rau ntim, thiab sib tov.
Chromatographic system (saib Chromatography 621)-Ua raws li qhia hauv Assay.Lub chromatograph yog programmed raws li hauv qab no.
Sijhawm (feeb) Tshuaj A (%) Tshuaj B (%) Elution
0–8 97 3 Ib
8-13 97®50 3®50 linear gradient
13–20 50 50 IB
20–25 50® 97 50®3 re-equilibration
Chromatograph cov kev daws teeb meem tsim nyog, thiab sau cov lus teb siab kawg raws li tau hais tseg rau Cov Txheej Txheem: lub sijhawm khaws cov txheeb ze yog kwv yees li 0.5 rau gemcitabine -anomer thiab 1.0 rau gemcitabine;qhov kev daws teeb meem, R, nruab nrab ntawm gemcitabine -anomer thiab gemcitabine tsis tsawg dua 8.0;thiab qhov tailing factor rau gemcitabine tsis ntau tshaj 1.5.Chromatograph tus qauv kev daws teeb meem, thiab sau cov lus teb ncov raws li tau hais tseg rau Cov Txheej Txheem: lub sijhawm khaws cov txheeb ze yog kwv yees li 0.1 rau cytosine thiab 1.0 rau gemcitabine;qhov txheeb ze tus qauv sib txawv rau kev txhaj tshuaj replicate tsis ntau tshaj 2.0%.
Txheej Txheem- Cais ib lub ntim (kwv yees li 20 µL) ntawm Standard tov thiab Test tov rau hauv chromatograph, sau cov chromatogram, thiab ntsuas tag nrho cov lus teb ncov.Xam qhov feem pua ​​​​ntawm cytosine hauv feem ntawm Gemcitabine coj los ntawm cov mis:
2.5 (Cc / W) (rt / rs)
nyob rau hauv uas Cc yog qhov concentration ntawm USP Cytosine RS nyob rau hauv Standard tov, nyob rau hauv µg ib mL;W yog qhov hnyav, hauv mg, ntawm Gemcitabine noj;rt yog lub ncov teb rau cytosine nyob rau hauv Test tov;thiab rs yog cov lus teb rau cytosine hauv Standard tov: tsis pub ntau tshaj 0.1% ntawm cytosine pom.Xam cov feem pua ​​​​ntawm txhua qhov impurity uas tsis yog cytosine hauv feem ntawm Gemcitabine coj los ntawm cov mis:
2.5 (Cs / W) (ri / rs)
nyob rau hauv uas Cs yog qhov concentration ntawm USP Gemcitabine Hydrochloride RS nyob rau hauv Standard tov, nyob rau hauv µg ib mL;W yog qhov hnyav, hauv mg, ntawm Gemcitabine noj;ri yog lub ncov teb rau txhua impurity nyob rau hauv lub Test tov;thiab rs yog cov lus teb vim gemcitabine nyob rau hauv Standard tov: tsis ntau tshaj 0.1% ntawm gemcitabine -anomer los yog lwm tus neeg impurity yog pom;thiab tag nrho cov impurities tsis ntau tshaj 0.2%.Tshem tawm ntawm tag nrho cov impurities ib qho peaks uas qis dua qhov kev txwv ntawm qhov ntau (0.02%).
Lwm qhov yuav tsum tau ua-Qhov twg daim ntawv lo hais tias Gemcitabine Hydrochloride yog tsis muaj menyuam, nws ua tau raws li qhov yuav tsum tau muaj rau cov kab mob endotoxins thiab Sterility raws li Gemcitabine rau Txhaj.Qhov twg daim ntawv lo hais tias Gemcitabine Hydrochloride yuav tsum tau ua ntxiv thaum lub sij hawm npaj cov tshuaj txhaj tshuaj, nws ua tau raws li qhov yuav tsum tau rau cov kab mob endotoxins nyob rau hauv Gemcitabine rau Txhaj.
Assay-
Txawb theem-Npaj lub lim thiab degassed tov uas muaj 13.8 g ntawm monobasic sodium phosphate thiab 2.5 mL ntawm phosphoric acid nyob rau hauv 1000 mL dej.[ceeb toom-Lub pH ntawm cov tshuaj no yog nyob nruab nrab ntawm 2.4 thiab 2.6.]
Kev tsim nyog rau kev daws teeb meem-Hloov txog 10 mg ntawm Gemcitabine Hydrochloride mus rau ib lub vial me me, ntxiv 4 mL ntawm cov tshuaj uas muaj 168 mg ntawm poov tshuaj hydroxide ib mL ntawm methanol, cap tightly, thiab sonicate.Thaum tshav kub kub ntawm 55 rau 6 mus rau 16 teev, cia kom txias, thiab hloov cov ntsiab lus mus rau 100-mL volumetric hwj nrog kev ntxuav ua tiav ntawm 1% (v / v) phosphoric acid.Dilute nrog 1% phosphoric acid rau ntim, thiab sib tov.[ceeb toom-Cov tshuaj no muaj txog 0.02 mg ib mL ntawm gemcitabine α-anomer.]
Cov txheej txheem kev npaj-Dissolve ib tug raug hnyav kom muaj nuj nqis ntawm USP Gemcitabine Hydrochloride RS nyob rau hauv dej, thiab dilute quantitatively, thiab stepwise yog tias tsim nyog, nrog dej kom tau txais ib tug paub concentration ntawm txog 0.1 mg ib mL.
Assay npaj-Hloov txog 20 mg ntawm Gemcitabine Hydrochloride, ntsuas kom raug, mus rau 200-mL ntim ntim, yaj hauv thiab dilute nrog dej rau ntim, thiab sib tov.
Chromatographic system (saib Chromatography <621>)-Cov kua chromatograph yog nruab nrog 275-nm detector thiab 4.6-mm × 25-cm kem uas muaj 5-µm packing L7.Tus nqi ntws yog li 1.2 mL ib feeb.Chromatograph qhov kev daws teeb meem tsim nyog, thiab sau cov lus teb siab tshaj plaws raws li qhia rau Cov Txheej Txheem: kev daws teeb meem, R, nruab nrab ntawm gemcitabine -anomer thiab gemcitabine tsis tsawg dua 8.0;thiab qhov tailing yam txiav txim los ntawm gemcitabine tsis ntau tshaj 1.5.Chromatograph tus txheej txheem npaj, thiab sau cov lus teb ncov raws li qhia rau Kev Ua Haujlwm: tus qauv sib txawv ntawm qhov sib txawv rau kev txhaj tshuaj tsis ntau tshaj 1.0%.
Cov txheej txheem-Kev txhaj tshuaj sib npaug (kwv yees li 20 µL) ntawm Cov Txheej Txheem Kev Npaj thiab Kev Ntsuas Kev Ntsuas rau hauv cov chromatograph, sau cov chromatograms, thiab ntsuas cov lus teb rau cov peaks loj.Xam qhov ntau, hauv mg, ntawm C9H11F2N3O4·HCl hauv feem ntawm Gemcitabine Hydrochloride coj los ntawm cov mis:
200C (rU / rS)
nyob rau hauv uas C yog qhov concentration, nyob rau hauv mg ib mL, ntawm USP Gemcitabine Hydrochloride RS nyob rau hauv tus txheej txheem npaj;thiab rU thiab rS yog cov lus teb siab kawg uas tau txais los ntawm Assay npaj thiab Standard npaj, feem.