I-D-Sorbitol CAS 50-70-4 Assay 97.0~100.5% Ikhwalithi ephezulu Yefektri

I-D-Sorbitol (CAS: 50-70-4) EP8.7 Indlela Yokuhlola
I-D-Glucitol (D-sorbitol).
Okuqukethwe: 97.0% ukuya ku-102.0% (into engenamanzi).
ABALINGISI
Ukubukeka: emhlophe noma ecishe ibe mhlophe, i-crystalline powder.
Ukunyibilika: kuncibilika kakhulu emanzini, cishe akuncibiliki ku-ethanol (amaphesenti angama-96).
Ibonisa i-polymorphism (5.9).
UKUDINTA
Umazisi wokuqala: A.
Ukuhlonza okwesibili: B, C, D
A. Hlola ama-chromatogram atholwe ekuhlolweni.
Imiphumela: ukuphakama okuyinhloko ku-chromatogram etholwe ngesixazululo sokuhlola kuyafana ngesikhathi sokugcinwa nosayizi kuya kunani eliphakeme kuchromatogram etholwe ngesixazululo sereferensi (a).
B. Chaza u-0.5 g ngokufudumeza enhlanganisweni engu-0.5 mL ye-pyridine Rand 5 mL ye-acetic anhydride R. Emva kwemizuzu eyi-10 thela ikhambi ku-25 mL wamanzi Irandi livumele lime emanzini anoqhwa amahora angu-2.Imvula, ekhiqizwe kabusha isuka kumthamo omncane we-ethanol (amaphesenti angama-96) R futhi yomiswa ku-vacuo, iyancibilika (2.2.14) ngo-98℃ ukuya ku-104℃.
C. I-chromatography yongqimba oluncane (2.2.27).
Isixazululo sokuhlola.Chaza u-25 mg wento ezohlolwa emanzini R bese uncibilikisa ibe ngu-10 ml ngesincibilikisi esifanayo.
Isixazululo sereferensi (a).Chaza u-25 mg we-sorbitol CRS emanzini R bese unciphisa ku-10 mL nge-solvent efanayo.
Isixazululo sereferensi (b).Chaza u-25 mg we-mannitol CRS kanye no-25 mg we-sorbitol CRS emanzini R bese unciphisa ku-10 mL nge-solvent efanayo.
Ipuleti: TLC silica gel G plate R.
Isigaba seselula: amanzi R, i-ethyl acetate R, i-propanol R (10:20:70V/V/V).
Isicelo: 2 μL
Ukuthuthukiswa: ngaphezu kwendlela ye-17cm
Ukomisa: emoyeni.
Ukutholwa: fafaza ngesisombululo se-4-aminobenzoic acid R;yomile emoyeni obandayo kuze kube yilapho i-acetone ikhishwa;ukushisa ku-100 ℃ imizuzu engu-15;vumela ukupholisa nokufutha ngesisombululo se-2g/L se-sodium periodate R;omile emoyeni obandayo;ukushisa ku-100 ℃ imizuzu engu-15.
Ukufaneleka kwesistimu: isixazululo sereferensi (b):
– ichromatogram ikhombisa 2 amabala ahlukaniswe ngokucacile.
Imiphumela: indawo eyinhloko kuchromatogram etholwe ngesixazululo sokuhlola iyafana ngokuma, umbala nosayizi nendawo eyinhloko kuchromatogram etholwe ngesixazululo sereferensi (a).
D. Ukujikeleza okuqondile kwe-optical (2.2.7): +4.0 kuya ku-+7.0 (i-anhydrou substance).
Chaza u-5.00 g wento ezohlolwa kanye no-6.4 g we-disodium tetraborate R ku-40 mL wamanzi R. Vumela ukuthi ime ihora elingu-1, unyakazise ngezikhathi ezithile, bese unciphisa ku-50.0mL ngamanzi R. Isihlungi uma kudingeka.
IZIVIVINYO
Ukubukeka kwesixazululo.Isixazululo sicacile(2.2.1) futhi asinambala (2.2.2, Indlela II).
Chaza u-5 g emanzini R bese unciphisa ku-50 mL nge-solvent efanayo.
I-Conductivity (2.2.38): umkhawulo ongu-20 μS·cm−1
Chaza u-20.0 g wamanzi angenayo i-incarbon dioxide R alungiswe emanzini agayiwe R bese uwanciphisa abe ngu-100.0 mL nge-solvent efanayo.Linganisa ukuqhutshwa kwesisombululo ngenkathi ushukumisa ngobumnene ngesishukumisi kazibuthe.
Ukunciphisa ushukela: okuphezulu ngamaphesenti angu-0.2, okuvezwa njengokulingana kweglucose.
Chaza u-5.0 g ku-6 mL wamanzi R ngosizo lokushisa okuthambile.Pholisa bese wengeza u-20 mL we-cupri-citric solution R kanye nobuhlalu obumbalwa bezingilazi.Shisisa ukuze ukubila kuqale ngemva kwemizuzu emi-4 bese uqhubeka ubila imizuzu emi-3.Pholisa ngokushesha bese wengeza u-100 mL wesisombululo esingu-2.4 samaphesenti angu-V/V se-glacial acetic acid R kanye no-20.0 mL we-iodine engu-0.025 M.Ngokunyakaziswa okuqhubekayo, engeza u-25 mL wengxube yemiqulu engu-6 ye-hydrochloric acid R kanye nevolumu engama-94 yamanzi R futhi, lapho imvula isincibilikile, cindezela i-iodine eyeqile ngo-0.05 M sodium thiosulfate usebenzisa i-1 mL ye-starch solution R, yengezwe. ngasekupheleni kwe-titration, njengenkomba.Kudingeka okungenani u-12.8 mL we-0.05 M sodium thiosulfate.
Izinto ezihlobene.I-chromatography yoketshezi(2.2.29).
Isixazululo sokuhlola.Chaza u-5.0 g wento okufanele ihlolwe ku-20 mL wamanzi R bese unciphisa ibe ngu-100.0 mL nge-solvent efanayo.
Isixazululo sereferensi (a).Chaza u-0.50g we-sorbitol CRS ku-2 mL wamanzi R futhi uhlambulule ube ngu-10.0 mL nge-solvent efanayo.
Isixazululo sereferensi (b).Nciphisa u-2.0mL wesixazululo sokuhlola sibe ngu-100.0 mL ngamanzi R.
Isixazululo sereferensi (c).Nciphisa u-5.0 mL wesixazululo sereferensi (b) siye ku-100.0 mL ngamanzi R.
Isixazululo sereferensi (d).Chaza u-0.5g we-sorbitol R no-0.5 g we-mannitol R (ukungcola A) ku-5 mL wamanzi R futhi uhlambulule ku-10.0 mL nge-solvent efanayo.
Ikholomu:
-usayizi:l=0.3m,Ø=7.8mm
-isigaba sokumisa: i-cation-exchange resin eqinile (ifomu le-calcium) R (9 μm);
-izinga lokushisa: 85±1°C
Isigaba sikamakhalekhukhwini: Amanzi acishiwe R.
Izinga lokugeleza: 0.5mL/min
Ukutholwa: i-refractometer igcinwe ezingeni lokushisa elingashintshi (isb. 35 °C).
Umjovo: 20μL wesisombululo sokuhlola nereferensi yezixazululo (b) (c) kanye (d)
Isikhathi sokusebenza: kabili isikhathi sokugcina se-sorbitol.
Ukugcinwa okuhlobene ngokubhekisela ku-sorbitol (isikhathi sokugcina = mayelana ne-27 min): ukungcola C = mayelana ne-0.6;ukungcola A = mayelana ne-0.8;ukungcola B = cishe 1.1.
Ukufaneleka kwesistimu: isixazululo sereferensi (d):
-ukulungiswa: ubuncane be-2.0 phakathi kweziqongo ngenxa yokungcola A ne-sorbitol.
Imikhawulo:
-noma yikuphi ukungcola: ngokungcola ngakunye, hhayi ngaphezu kwendawo yokuphakama okuyinhloko ku-chromatogram etholwe ngesixazululo sereferensi (b) (amaphesenti angu-2);
-inani: izikhathi ezingeqi kwezingu-1.5 endaweni yesiqongo esiyinhloko kuchromatogram etholwe ngesixazululo sereferensi (b) (3 amaphesenti);
-umkhawulo wokunganaki: indawo yenani eliphakeme eliyinhloko kuchromatogram etholwe ngesixazululo sereferensi (c) (amaphesenti angu-0.1).
Ukuhola (2.4.10): umkhawulo ongu-0.5 ppm.
I-Nickel (2.4.15): umkhawulo ongu-1 ppm.
Chaza into ezohlolwa ku-150.0 mL wengxube enqunyiwe yezincibilikisi.
Amanzi (2.5.12): isilinganiso esiphezulu samaphesenti angu-1.5, anqunywa ku-1.00 g.Sebenzisa ingxube yevolumu engu-1 ye-formamide R kanye namavolumu angu-2 we-anhydrous methanol R njengesinyibilikisi.
Ukungcoliswa kwamagciwane
Uma ihloselwe ukusetshenziswa ekwenzeni amalungiselelo parenteral:
– TAMC: umbandela wokwamukela 102CFU/g (2.6.12).
Uma kungahloselwe ukusetshenziswa ekwenzeni amalungiselelo omzali:
– TAMC: umbandela wokwamukela 103CFU/g (2.6.12);
– I-TYMC: umbandela wokwamukela i-102CFU/g (2.6.12);
-ukungabikho kwe-Escherichia coli (2.6.13);
-ukungabikho kweSalmonella (2.6.13).
Ama-endotoxin amagciwane (2.6.14).Uma kuhloswe ukuthi kusetshenziswe ekwenzeni amalungiselelo omzali ngaphandle kwenqubo efanelekile yokususwa kwe-endotoxin yebhaktheriya:
- ngaphansi kwe-4 IU/g yamalungiselelo omzali ane-concentration engaphansi kwe-100g/L ye-sorbitol
- ngaphansi kwe-2.5 IU/g yamalungiselelo ama-parenteral ane-concentration ye-100g/L noma ngaphezulu ye-sorbitol
ISIVIVINYO
I-Liquid chromatography (2.2.29) njengoba kuchazwe ekuhlolweni kwezinto ezihlobene nokuguqulwa okulandelayo.
Umjovo: isixazululo sokuhlola nesixazululo sereferensi (a).
Bala iphesenti lokuqukethwe kwe-D-sorbitol kusukela kokuqukethwe okumenyezelwe kwe-sorbitol CRS.
LABELING
Ilebula ithi:
- lapho kufanele khona, ukugcwala okuphezulu kwama-endotoxins ebhaktheriya;
– lapho kufanele khona, ukuthi into ifanele ukusetshenziswa lapho kwenziwa amalungiselelo omzali.
UKUNGCOLA
A. D-mannitol,
B. D-iditol,
C. 4-O-α-D-glucopyranosyl-D-glucitol (D-maltitol).

I-D-Sorbitol (CAS: 50-70-4) Indlela Yokuhlola ye-USP
INCAZELO
I-Sorbitol iqukethe i-NLT 91.0% ne-NMT 100.5% ye-D-sorbitol, ibalwe ngesisekelo se-anhydrous.Amanani engqikithi kashukela, obunye obunama-polyhydric alcohols, nanoma iyiphi i-hexitol anhydrides, uma etholiwe, awafakiwe ezidingweni, noma enanini elibaliwe ngaphansi Kokunye Ukungcola Ezazisweni Ezivamile.
UKUKHOMBA
• A.
Isixazululo sesampula: 1g ye-Sorbitol ku-75 mL wamanzi
Ukuhlaziya: Dlulisa u-3 mL wesixazululo Sesampula eshubhuni yokuhlola engu-15-cm, bese wengeza u-3 mL wesixazululo secatechol esisanda kulungiswa (1 ku-10), bese uxuba.Engeza u-6 mL we-sulfuric acid, bese ushisisa kancane ishubhu elangabini lamasekhondi angu-30.
• B. Isikhathi sokugcina sesiqongo esikhulu sesixazululo Sesampuli sihambisana nalokho okuvela kusixazululo Esijwayelekile, njengoba kutholwe ku-Assay.
ISIVIVINYO
• INQUBO
Isigaba sikamakhalekhukhwini: Sebenzisa amanzi akhishwe umoya.
Isixazululo sokufaneleka kwesistimu: Lungiselela isixazululo esiqukethe u-4.8 mg/g we-USP ngayinye ye-Sorbitol RS kanye ne-mannitol
Isixazululo esijwayelekile: 4.8 mg/g ye-USP Sorbitol RS
Isixazululo sesampula: Chaza i-0.10 g ye-Sorbitol emanzini, bese uhlanza ngamanzi ukuya ku-20g.Qopha isisindo sokugcina sesixazululo, bese uxuba kahle.
Isistimu yeChromatographic
(Bona i-Chromatography <621>, Ukufaneleka Kwesistimu.)
Imodi: LC
Umtshina: Inkomba ye-Refractive
Ikholomu: 7.8-mm x 10-cm;ukupakisha L34
Izinga lokushisa
Ikholomu: 50±2°
Umtshina: 35°
Izinga lokugeleza: 0.7 mL/min
Usayizi womjovo: 10 μL
Ukufaneleka kwesistimu
Amasampula: Isixazululo sokufaneleka kwesistimu nesixazululo Esijwayelekile [QAPHELA-Izikhathi zokugcinwa okuhlobene kwe-mannitol ne-sorbitol cishe zingu-0.6 no-1.0, ngokulandelana.]
Izidingo zokufaneleka
Isixazululo: I-NLT 2.0 phakathi kwe-sorbitol ne-mannitol, isisombululo sokufaneleka kwesistimu
Ukuchezuka okujwayelekile okuhlobene: I-NMT 2.0%, Isixazululo esijwayelekile
Ukuhlaziya
Amasampula: Isixazululo esijwayelekile kanye nesixazululo esiyisampula
Bala iphesenti, ngesisekelo se-anhydrous, ye-D-sorbitol engxenyeni ye-Sorbitol ethathiwe:
Umphumela = (rU/rS) x (CS/CU) x (100/(100 -W)) x 100
rU= impendulo ephezulu evela kusixazululo Sesampula
rS= impendulo ephezulu evela kusixazululo Esijwayelekile
CS= ukugxila kwe-USP Sorbitol RS kusixazululo Esijwayelekile (mg/g)
CU= ukugcwala kwe-Sorbitol kusixazululo Sesampula (mg/g)
W= iphesenti elitholwe ekuhlolweni kokunqunywa kwamanzi
Imibandela yokwamukela: 91.0%–100.5% ngesisekelo esingenamanzi
UKUNGCOLA
• UMKHAWULO WE-NICKE
Isixazululo sesampula: Chaza u-20.0 g we-Sorbitol ku-acetic acid ehlanjululwe, bese uhlanjululwa nge-acetic acid ehlanjululwe ku-150 mL.
Isixazululo esingenalutho: 150 mL we-acetic acid ehlanjululwe
Izisombululo ezijwayelekile: Lungiselela izixazululo ezintathu ngokungeza u-0.5, 1.0, kanye no-1.5 mL we-nickel standard solution TS ku-20.0 g we-Sorbitol encibilikisiwe ku-acetic acid ehlanjululwe, bese uhlanjululwa nge-solvent efanayo ku-150 mL.
Izimo zezinsimbi
(Bheka i-Spectrophotometry and Light-scattering <851>)
Imodi: I-spectrophotometry yokumuncwa kwe-athomu
Ubude begagasi bokuhlaziya: 232.0 nm
Isibani: i-nickel hollow-cathode
Ilangabi: I-Air-acetylene
Ukuhlaziya
Amasampula: Izisombululo ezijwayelekile kanye nesixazululo esiyisampula
Kusampula ngayinye engeza u-2.0 mL wesixazululo se-ammonium pyrrolidinedithiocarbamate esigcwele (esiqukethe u-10g/L we-ammonium pyrrolidinedithiocarbamate) no-10.0 mL we-methyl isobutyl ketone, bese unyakazisa amasekhondi angu-30.Vikela ekukhanyeni okukhanyayo.Vumela izendlalelo ezimbili ukuthi zihlukane, bese usebenzisa isendlalelo se-methyl isobutyl ketone.Setha ithuluzi libe uziro usebenzisa isendlalelo se-organic kusuka kusixazululo Esingenalutho.
Ngokuhambisanayo thola ukumunca kongqimba lwemvelo kusuka Kumasampuli okungenani izikhathi ezintathu lilinye.Rekhoda isilinganiso sokufundwa okungaguquguquki kwesixazululo ngasinye Esijwayelekile kanye nesixazululo Sesampuli.Phakathi kwesilinganiso ngasinye, langazelela isendlalelo se-organic kusuka kusixazululo Esingenalutho, futhi uqinisekise ukuthi ukufundwa kubuyela ku-zero.Hlela ukumuncwa kwezixazululo Ezijwayelekile kanye nesixazululo Sesampula ngokumelene nenani elengeziwe le-nickel.
Yengeza umugqa ohlanganisa amaphuzu kugrafu uze uhlangane ne-eksisi yokugxilisa ingqondo.Ibanga eliphakathi kwaleli phuzu nokuphambana kwezimbazo limelela ukugxiliswa kwe-nickel kusixazululo Sesampuli.
Imibandela yokwamukela: NMT 1 ppm
• UKUSHISA OKUSELELE <281>: I-NMT 0.1%, kunqunywa engxenyeni engu-1.5g
UKWEHLISA USHUKELA
[QAPHELA-Inani elinqunywe kulokhu kuhlolwa alifakiwe enanini elibaliwe ngaphansi Kokunye Ukungcola Ezazisweni Ezivamile.]
Isixazululo esiyisampula: Chaza u-3.3 g we-Sorbitol ku-3 mL wamanzi ngosizo lokushisa okuthambile.Phola, bese wengeza u-20.0 mL we-cupric citrate TS kanye nobuhlalu obumbalwa bezingilazi.Shisisa ukuze ukubila kuqale ngemva kwemizuzu emi-4, bese uqhubeka ubila imizuzu emi-3.Phola ngokushesha, bese wengeza u-40 mL we-acetic acid ehlanjululwe, u-60 mL wamanzi, kanye no-20.0 mL we-0.05 N iodine VS.Ngokunyakazisa okuqhubekayo, engeza u-25 mL wengxube ka-6 mL we-hydrochloric acid kanye nama-94 mL amanzi.
Ukuhlaziywa: Uma imvula isincibilikile, cindezela ukweqisa kwe-iodine nge-0.05 N sodium thiosulfate VS usebenzisa u-2mL wesitashi TS, wengezwe ngasekupheleni kwe-titration, njengenkomba.
Imibandela yokwamukela: I-NLT 12.8 mL ka-0.05 N sodium thiosulfate VS iyadingeka, ehambisana ne-NMT 0.3% yokwehlisa ushukela, njengeglucose
• I-CHLORIDEAND SULFATE, I-Chloride<221> (uma inelebuli yokusetshenziswa ekulungiseleleni amafomu omthamo wabazali)
Isampula: 1.5 g
Imibandela yokwamukela: Isampuli ayibonisi i-chloride eningi kunaleyo ehambelana no-0.10 mL ka-0.020 N hydrochloric acid (NMT 0.0050%).
• I-CHLORIDEAND SULFATE, i-Sulfate <221> (uma inelebuli yokusetshenziswa ekulungiseleleni amafomu omthamo wabazali)
Isampula: 1.0 g
Imibandela yokwamukela: Isampuli ayibonisi i-sulfate eningi kunokuhambisana no-0.10 mL ka-0.020 N sulfuric acid (NMT 0.01%).
IZIVIVINYO EZITHILE
• IZIVIVINYO ZOKUBALA I-MICROBIAL <61> kanye IZIVIVINYO ZEMICROORGANISMS Ecacisiwe <62>: Isamba sesibalo se-aerobic sisebenzisa i-Plate Method yi-NMT 1000 cfu/g, futhi isamba sesibalo sesikhunta neyeast esihlanganisiwe yi-NMT 100 cfu/g
• PH <791>: 3.5-7.0, kusixazululo esingu-10% (w/w) emanzini angenayo i-carbon dioxide
• UKUNIKEZWA KWAMANZI, Indlela I <921>: I-NMT 1.5%
I-CLARITYAND COLOROF SOLUTION(uma inelebuli yokusetshenziswa ekulungiseleleni amafomu omthamo wabazali)
Isampula: 10.0 g
Ukuhlaziya: Chaza Isampula ku-100.0 mL wamanzi angenayo i-carbon dioxide.
Indlela yokwamukela: Isixazululo sicacile futhi asinambala.
• ISIVIVINYO SAMA-Endotoxin Amagciwane <85> (uma alebulwe ukuthi asetshenziswe ekulungiseleleni amafomu omthamo womzali): I-NMT 4 USP Endotoxin Units/g yamafomu omthamo wabazali anokuhlangana okungaphansi kuka-100g/L we-sorbitol, kanye ne-NMT 2.5 USP Endotoxin Units/g kumafomu omthamo we-parenteral ane-concentration ye-100g/L noma ngaphezulu ye-sorbitol.
IZIDINGO EZENGEZIWE
• PACKAGINGAND STORAGE: Londoloza ezitsheni ezivalwe kahle.Azikho izidingo zesitoreji ezishiwo.
• UKULEBULA: I-Sorbitol ehloselwe ukusetshenziswa ekulungiseleleni amafomu emithamo yabazali ibhalwe kanjalo.
I-USP REFERENCE AMAZINGA <11>
USP Endotoxin RS
I-USP Sorbitol RS