I-SBE-β-CD CAS 182410-00-0 Betadex Sulfobutyl Ether Sodium Assay 95.0~105.0%

I-Betadex Sulfobutyl Ether Sodium
C42H70−nO35 · (C4H8SO3Na)n 2163 lapho n = 6.5
I-Beta cyclodextrin sulfobutyl ethers, usawoti we-sodium;
I-Beta cyclodextrin sulfobutyl ether sodium [182410-00-0].
INCAZELO
I-Betadex Sulfobutyl Ether Sodium ilungiswa nge-alkylation ye-betadex kusetshenziswa i-1,4-butane sultone ngaphansi kwezimo eziyisisekelo.
Izinga elimaphakathi lokushintsha ku-betadex yi-NLT 6.2 kanye ne-NMT 6.9.
Iqukethe i-NLT 95.0% kanye ne-NMT 105.0% ye-C42H70−nO35 · (C4H8SO3Na)n (n = 6.2–6.9), ibalwe ngesisekelo se-anhydrous.
UKUKHOMBA
• A. UKUMUMVA OKUNOMTHWALO <197K>
• B. Isikhathi sokugcina sesiqongo esikhulu sesixazululo Sesampuli sihambisana naleso sesixazululo esijwayelekile, njengoba sitholwe ku-Assay.
• C. Ihlangabezana nezimfuneko zokuhlolwa kwe-Average Degree of Substitution.
• IZIVIVINYO ZOKUKHOMBA JIKELELE, I-Sodium 〈191〉
ISIVIVINYO
• INQUBO
Isigaba seselula: 0.1 M potassium nitrate engxubeni ye-acetonitrile namanzi (1:4)
Isixazululo esijwayelekile: 10 mg/mL ye-USP Betadex Sulfobutyl Ether Sodium RS esigabeni Seselula
Isixazululo sesampula: 10 mg/mL we-Betadex Sulfobutyl Ether Sodium esigabeni se-Mobile
Isistimu yeChromatographic
(Bona i-Chromatography <621>, Ukufaneleka Kwesistimu.)
Imodi: LC
Umtshina: Inkomba ye-Refractive
Izinga lokushisa lomtshina: 35 ± 2°
Ikholomu: 7.8-mm × 30-cm ikholomu yokuhlaziya;ukupakisha L37.[QAPHELA-Geza ikholomu ngesixazululo se-acetonitrile namanzi (1:9) ekuqedeni uchungechunge olusebenzayo.]
Izinga lokugeleza: 1.0 mL/min
Usayizi womjovo: 20 µL
Ukufaneleka kwesistimu .
Isampula: Isixazululo esijwayelekile
Izidingo zokufaneleka
Ukuchezuka okujwayelekile okuhlobene: NMT 2.0%
Ukuhlaziya
Amasampula: Isixazululo esijwayelekile kanye nesixazululo esiyisampula
Bala iphesenti le-betadex sulfobutyl ether sodium [C42H70−nO35 · (C4H8SO3Na)n] engxenyeni ye-Betadex Sulfobutyl Ether Sodium ethathiwe:
Umphumela = (rU/rS) × (CS/CU) × 100
rU = impendulo ephezulu ye-betadex sulfobutyl ether
i-sodium kusuka kusixazululo sesampula
rS = impendulo ephezulu ye-betadex sulfobutyl ether
sodium kusuka kusixazululo Esijwayelekile
CS = ukugxila kwe-USP Betadex Sulfobutyl Ether
I-Sodium RS kusixazululo Esijwayelekile (mg/mL)
CU = ukuhlushwa kwe-Betadex Sulfobutyl Ether Sodium kusixazululo Sesampula (mg/mL)
Indlela yokwamukela: 95.0%~105.0% kusisekelo se-anhydrous
UKUNGCOLA
• IZIMTHETHO EZISINDAYO, Indlela II <231>: NMT 5 ppm
• UMKHAWULO WE-BETA CYCLODEXTRIN (BETADEX)
Isixazululo A: 25 mM sodium hydroxide
Isixazululo B: 250 mM sodium hydroxide kanye 1 M potassium nitrate
Isigaba sikamakhalekhukhwini: Bheka Ithebula 1.
Ithebula 1

Isixazululo esijwayelekile: 2 µg/mL ye-USP Beta Cyclodextrin RS
Isixazululo sesampula: 2 mg/mL we-Betadex Sulfobutyl Ether Sodium
Isistimu yeChromatographic
(Bona i-Chromatography <621>, Ukufaneleka Kwesistimu ne-Ion Chromatography <1065>.)
Imodi: IC
Umtshina: I-amperometry eshayekile (iseli ye-amperometric ene-electrode esebenzayo yegolide kanye ne-electrode eyireferensi yesiliva)
Ikholomu
Umqaphi: 4.0-mm × 5-cm anion-exchange;ukupakisha L61
Ukuhlaziya: 4.0-mm × 25-cm anion-exchange;
ukupakisha L61
Izinga lokushisa lekholomu: 50 ± 2°
Izinga lokugeleza: 1.0 mL/min
Usayizi womjovo: 20 µL
I-Waveform ye-pulsed amperometric detector: Bheka Ithebula 2.
Ithebula 2

Ukufaneleka kwesistimu
Isampula: Isixazululo esijwayelekile
Izidingo zokufaneleka
Ukuchezuka okujwayelekile okuhlobene: NMT 5.0%
Ukuhlaziya
Amasampula: Isixazululo esijwayelekile kanye nesixazululo esiyisampula
Bala iphesenti le-beta cyclodextrin (betadex) engxenyeni ye-Betadex Sulfobutyl Ether Sodium ethathiwe:
Umphumela = (rU/rS) × (CS/CU) × F × 100
rU = impendulo ephakeme kakhulu ye-beta cyclodextrin evela kusixazululo Sesampula
rS = impendulo ephezulu ye-beta cyclodextrin evela kusixazululo Esijwayelekile
CS = ukugxila kwe-USP Beta Cyclodextrin RS kusixazululo Esijwayelekile (µg/mL)
CU = ukuhlushwa kwe-Betadex Sulfobutyl Ether Sodium kusixazululo Sesampula (mg/mL)
F = isici sokuguqula (10-3 mg/µg)
Imibandela yokwamukela: NMT 0.1%
• UMKHAWULO KA-1,4-BUTANE SULTONE
Isixazululo esijwayelekile sangaphakathi: 0.25 µg/mL ye-diethyl sulfone
Isixazululo esijwayelekile sesitoko A: 0.5 µg/mL ye-1,4-butane sultone
Isixazululo esijwayelekile sesitoko B: 1.0 µg/mL ye-1,4-butane sultone
Isixazululo sesitoko esijwayelekile C: 2.0 µg/mL se-1,4-butane sultone
Isixazululo sesitoko esiyisampula: 250 mg/mL we-Betadex Sulfobutyl Ether Sodium kusixazululo esijwayelekile sangaphakathi
Isixazululo esingenalutho, kanye nesampula yezixazululo A, B, C, kanye no-D:
Landela Ithebula lesi-3 ukuze ubeke amanani esixazululo esijwayelekile sangaphakathi, isisombululo ngasinye sesitoko Esijwayelekile, isampula yesixazululo sesitoko, amanzi, noma i-methylene chloride kushubhu ngayinye yokuhlola ingilazi enesivalo.[QAPHELA-I-screw-capped, ishubhu lokuhlola elingu-10-mL lifanelekile.] Xuba kumxube we-vortex ityhubhu ngalinye lokuhlola amasekhondi angu-30, futhi ulivumele lime okungenani imizuzu emi-5 noma kuze kuhlukaniswe ngokuphelele isigaba.Khipha isigaba se-organic ku-vial ye-GC bese uvala.[QAPHELA-Ngokucophelela thatha inani elincane elingenzeka lesigaba samanzi.] Amanani angeziwe we-1,4-butane sultone kuzixazululo zesampula A, B, C, kanye no-D ngu-0.5, 1.0, 2.0, kanye no-0 µg, ngokulandelanayo.
Ithebula 3

[QAPHELA-Lungiselela ngokushesha ngaphambi kokusebenzisa.]
Isistimu yeChromatographic
(Bona i-Chromatography <621>, Ukufaneleka Kwesistimu.)
Imodi: GC
Umtshina: I-ionization yomlilo
Ikholomu: 0.32-mm × 25-m fused-silica capillary ikholomu;0.5-µm isendlalelo sesigaba G46
Izinga lokushisa
Umtshina: 270°
Imbobo yomjovo: 200°
Ikholomu: Bona uhlelo lwezinga lokushisa kuThebula 4
Ithebula 4
Ithempelesha Yokuqala (°) Irempu Yezinga lokushisa (°/min) Ithempelesha Yokugcina (°) Ukubamba Isikhathi Emazingeni Okushisa Okugcina (min)
100 10 200 -
200 35 270 5
Igesi yenkampani yenethiwekhi: I-Helium, ngokuvamile i-12 psi inlet pressure
Usayizi womjovo: 1.0 µL
Uhlobo lomjovo: Umjovo ongena-splitless imizuzu engu-0.5, bese uhlukaniswa ngo-50 mL/min.[QAPHELA-Kunconywa ukusetshenziswa komugqa womjovo ongahlukanisiwe ofanelekile.]
Ukufaneleka kwesistimu
Isampula: Isampula yesixazululo B
[QAPHELA-Izikhathi zokugcinwa okuhlobene ze-diethyl sulfone ne-1,4-butane sultone zingu-0.7 kanye no-1.0, ngokulandelanayo.]
Izidingo zokufaneleka
Ukuchezuka okujwayelekile okuhlobene: NMT 10.0%
Ukuhlaziya
Amasampula: Isixazululo esingenalutho, izixazululo zesampula A, B, C, kanye no-D
Lungisa isilinganiso sezimpendulo eziphezulu ze-1,4-butane sultone ku-diethyl sulfone kusixazululo sesampuli A, B, C, noma D ngokukhipha isilinganiso sezimpendulo eziphezulu ze-1,4-butane sultone ku-ethyl sulfone kusixazululo Esingenalutho. .Hlela isilinganiso esilungisiwe sokuphendula okuphezulu kwe-1,4-butane sultone ekuphenduleni okuphezulu kwe-diethyl sulfone kusixazululo Sesampuli A, B, C noma D, uma kuqhathaniswa nenani elingeziwe, ku-µg, le-sultone engu-1,4-butane.Yengeza umugqa ohlanganisa amaphuzu kugrafu uze uhlangane ne-eksisi yobuningi.Ibanga eliphakathi kwaleli phuzu nokuphambana kwezimbazo limelela inani le-1,4-butane sultone, A, ku-µg, engxenyeni engu-4-mL yesisombululo sesitoko.Bala okuqukethwe kwe-1,4-butane sultone engxenyeni ye-Betadex Sulfobutyl Ether Sodium ethathiwe:
Umphumela = A/(VExt × CU × F)
A = kunqunywa ngenhla
I-VExt = umthamo wesixazululo sesitoko esiyisampula esisetshenziswe esinyathelweni sokukhipha, 4.0 mL
I-CU = ukuhlushwa kwe-Betadex Sulfobutyl Ether Sodium kusixazululo sesitoko Sesampula (mg/mL)
F = isici sokuguqula (10-3 g/mg)
Indlela yokwamukela: i-hydroxybutane-1-sulfonic acid, noma i-NMT 0.5 ppm
• UMKHAWULO WESODIUM CHLORIDE, 4-HYDROXYBUTANE-1-SULFONIC ACID, KANYE NE-BIS(4-SULFOBUTYL) ETHER DISODIUM
Isixazululo A: I-5 mM i-sodium hydroxide, i-degas emkhunjini ovaliwe we-15 min
Isixazululo B: 25 mM sodium hydroxide, i-degas emkhunjini ovaliwe we-15 min
Isigaba sikamakhalekhukhwini: Bheka Ithebula 5
Ithebula 5

Isixazululo sokugeza ikholomu A: 50 mM sodium citrate
Isixazululo sokugeza ikholomu B: 150 mM i-sodium hydroxide
Isixazululo esijwayelekile: Lungiselela isixazululo esinokugxilisa okwaziwayo okungu-8 µg/mL kwe-USP Sodium Chloride RS, 4µg/mL ye-4-hydroxybutane-1-sulfonic acid, kanye no-4 µg/mL we-bis(4-sulfobutyl) ether disodium.
Isixazululo sesampula: 4 mg/mL ye-Betadex Sulfobutyl Ether Sodium
Isistimu yeChromatographic
(Bona i-Chromatography <621>, Ukufaneleka Kwesistimu ne-Ion Chromatography <1065>.)
Imodi: IC
Umtshina: I-Conductivity
Ibanga: 30 µS
Okwamanje: 100 mA
Ikholomu: [QAPHELA-Ekugcineni kokugijima ngakunye, hlanza ikholomu usebenzisa isisombululo sokugeza Ikholomu A ngesilinganiso sokugeleza esingu-1 mL/min imizuzu engama-35 bese usebenzisa isixazululo sokugeza Ikholomu B ngesilinganiso sokugeleza esifanayo semizuzu engama-35.]
Umqaphi: 4.0-mm × 5.0-cm anion-exchange;ukupakisha L61
Ukuhlaziya: 4.0-mm × 25-cm anion-exchange;ukupakisha L61
Izinga lokushisa lekholomu: 30°
Umcindezeli: I-Micromembrane anion autosuppressor1 noma uhlelo olufanele lokucindezela amakhemikhali
Ukucindezela: Ukucindezela okuzenzakalelayo
Izinga lokugeleza: 1.0 mL/min
Usayizi womjovo: 20 µL
Ukufaneleka kwesistimu
Isampula: Isixazululo esijwayelekile
[QAPHELA-Izikhathi zokugcinwa okuhlobene zinikezwe ulwazi kuphela.Izikhathi zokugcinwa okuhlobene ze-4-hydroxybutane-1-sulfonate ion, chloride ion, ne-bis(sulfobutyl) ether ion ngu-1.0, 1.4, kanye no-8.6, ngokulandelana.]
Izidingo zokufaneleka
Isixazululo: NLT 2.0
Ukuchezuka okujwayelekile okuhlobene: NMT 10.0%
Ukuhlaziya
Amasampula: Isixazululo esijwayelekile kanye nesixazululo esiyisampula
Bala iphesenti le-sodium chloride, 4-hydroxybutane-1-sulfonic acid, noma i-bis(sulfobutyl) ether disodium engxenyeni ye-Betadex Sulfobutyl Ether Sodium ethathiwe:
Umphumela = (rU/rS) × (CS/CU) × F × 100
i-rU = impendulo ephezulu ye-sodium chloride, i-4-hydroxybutane-1-sulfonic acid, noma i-bis(sulfobutyl) ether disodium evela kusixazululo Sesampula
rS = impendulo ephezulu ye-sodium chloride, i-4-hydroxybutane-1-sulfonic acid, noma i-bis(sulfobutyl) ether disodium evela kusixazululo Esijwayelekile
CS = ukuhlushwa kwe-sodium chloride, 4-hydroxybutane-1-sulfonic acid, noma i-bis(sulfobutyl) ether disodium kusixazululo Esijwayelekile (µg/mL)
CU = ukuhlushwa kwe-Betadex Sulfobutyl Ether Sodium kusixazululo Sesampula (mg/mL)
F = isici sokuguqula (10−3 0 100 0 mg/µg)
Imibandela yokwamukela
I-sodium chloride: NMT 0.2%
4-Hydroxybutane-1-sulfonic acid: NMT 0.09%
I-Bis(sulfobutyl) ether disodium: NMT 0.05%
IZIVIVINYO EZITHILE
UKUHLOLWA KWE-BACTERIAL ENDOTOXINS <85>: Izinga lama-endotoxins ebhaktheriya liwukuthi imfuneko ngaphansi kwefomu lesilinganiso esifanelekile se-monograph(s) lapho kusetshenziswa i-Betadex Sulfobutyl Ether Sodium ingahlangatshezwana nayo.Lapho ilebula ithi i-Betadex Sulfobutyl Ether Sodium kumele ibe ngaphansi kokucubungula okwengeziwe ngesikhathi sokulungiswa kwamafomu omthamo omjovo, izinga le-endotoxin yebhaktheriya liwukuthi imfuneko ngaphansi kwefomu lomthamo ofanele we-monograph(s) lapho kusetshenziswa i-Betadex Sulfobutyl Ether Sodium. kungahlangatshezwana nazo.
• IZIVIVINYO ZOKUBALA I-MICROBIAL <61> kanye IZIVIVINYO ZEMICROORGANISMS Ecacisiwe <62>: Isamba sesibalo se-aerobic microbial asidluli ku-100 cfu/g, futhi isamba sesibalo sesikhunta esihlanganisiwe neyeast asidluli ku-50 cfu/g.Ihlangabezana nezimfuneko zokuhlolwa kokungabikho kwe-Escherichia coli.
• UKUCACA KWESIXAZULULO
Isixazululo sesampula: 30% (w/v) isisombululo
Ukuhlaziya: Hlola isixazululo Sesampuli usebenzisa ibhokisi elikhanyayo ngokumelene nengemuva elimhlophe nelimnyama, bese ubhala ukuba khona kwanoma iyiphi inkungu, i-fluorescence, imicu, ama-specks, noma enye into yangaphandle.
Indlela yokwamukela: Isixazululo sicacile, futhi empeleni asinazo izinhlayiya zodaba lwangaphandle.
• I-Avareji IDIGRI LOKUSHINTSHA
Qalisa i-electrolyte: 30 mM benzoic acid futhi ilungiselwe i-pH efanele ithuluzi elisetshenziswa ngokungezwa kwe-100 mM tris(hydroxymethyl) aminomethane buffer.
[QAPHELA-Ngenxa yokuhluka phakathi kwama-capillary, i-pH eyodwa ye-electrolyte esebenza emhlabeni wonke ayicacisiwe.
Esikhundleni salokho, i-pH elungile ehambisana ne-capillary ngayinye kufanele inqunywe ngokuya ngemanuwali yezinsimbi.]
Isixazululo esijwayelekile: 10 mg/mL ye-USP Betadex Sulfobutyl Ether Sodium RS
Isixazululo sesampula: 10 mg/mL ye-Betadex Sulfobutyl Ether Sodium
Inqubo yokuhlanza i-capillary: Sebenzisa izitsha ezihlukene ze-electrolyte ukuze uhlanza i-capillary kanye nokuhlaziya isampula.Yenza uhlaziyo lwangaphambi kokuhlaziya nsuku zonke ngaphambi kokuhlaziya ngakunye: hlambulula i-capillary nge-0.1 N sodium hydroxide imizuzu engu-30, ngamanzi e-NLT 2 h, kanye ne-Run electrolyte ye-NLT 1 ihora.Hlanza ngaphambi kokujova ngaphambi komjovo ngamunye ngale ndlela elandelayo.Hlanza i-capillary nge-0.1 N sodium hydroxide ye-NLT 1 iminithi, kanye ne-Run electrolyte for NLT 3 min.Uma kusetshenziswa i-capillary entsha, ngaphezu kwama-rinses avamile achazwe ngenhla, i-capillary entsha idinga ukugeza ngaphambi kokusetshenziswa kwayo kokuqala.Hlanza i-capillary entsha nge-1 M sodium hydroxide ihora elingu-1, kulandele ukugeza kwamanzi amahora angu-2.
Isistimu ye-Electrophoretic
(Bheka i-Capillary Electrophoresis <1053>.)
Imodi: Ukusebenza okuphezulu kwe-CE
Umtshina: I-UV ephambene engu-200 nm, enomkhawulokudonsa ongu-20nm.[QAPHELA-Ukutholwa kwe-wavelength engu-205 nm enomkhawulokudonsa ongu-10 nm kungase kusetshenziswe njengenye indlela.]
Ikholomu: I-Sodium Peaks I–X (% Indawo Ephakeme) 50-µm × 50-cm ikholomu yesilika ehlanganisiwe
Izinga lokushisa lekholomu: 25°
Amandla kagesi asetshenziswayo: 0.00 kuye +30.00 kV irempu yomugqa ngaphezu kwemizuzu eyi-10, bese kuba ku-30 ​​kV eminye imizuzu engama-20
Usayizi womjovo: Amavolumu alinganayo ku-0.5 psi amasekhondi ayi-10
Ukufaneleka kwesistimu
Isampula: Isixazululo esijwayelekile
[QAPHELA-Bheka Ithebula 6 mayelana nezikhathi zokufuduka kwesihlobo esilinganiselwe se-betadex sulfobutyl ether sodium peaks I–X (i-betadex sulfobutyl ether sodium peaks I, II, III, ..., X, iqukethe i-beta cyclodextrin molecule ene-1, 2, 3, ..., 10 sulfobutyl substituent(ama), ngokulandelana).Izikhathi zokufuduka okuhlobene ezezinjongo zolwazi kuphela ukusiza ekukhombeni okuphezulu.]
Ithebula 6

Izidingo zokufaneleka
Ukulungiswa: NLT 0.9, phakathi kwe-betadex sulfobuty ether sodium peak IX kanye ne-betadex sulfobutyl ether sodium peak X
Ukuhlaziya
Amasampula: Qalisa i-electrolyte, amanzi, isixazululo esijwayelekile, kanye nesixazululo sesampula
Jova isisombululo Esijwayelekile kanye nesixazululo Sesampuli ngokusebenzisa ingcindezi ehlukile engu-0.5 psi, okulingana no-34 mbar, amasekhondi angu-10, okulandelwa umjovo we-Run electrolyte ku-0.5 psi amasekhondi angu-2.[QAPHELA-Imijovo yokucindezela kufanele yenziwe ngebhodlela lamanzi noma Run electrolyte ekugcineni kwe-capillary.]
Rekhoda ama-electropherogram, bese ukala izimpendulo eziphezulu ze-betadex sulfobutyl ether sodium peaks (I ukuya ku-X).Bala indawo ephakemeyo elungisiwe, i-AI, yesiqongo ngasinye ku-eletropherogram:
Indawo Ephakeme Elungisiwe A = Indawo Ephakeme x Ubude be-Capillary obusebenzayo (cm) / Isikhathi Sokufuduka
Hlela izindawo eziphakeme ezilungisiwe ngokwethula ngayinye njengephesenti lengqikithi yendawo yemvilophu elungisiwe:
Indawo Emisiwe, NA: A / n∑i=1 Ai x 100
n = izinga eliphezulu lokushintsha
Nquma idigri emaphakathi yokufaka esikhundleni:
I-Average Degree of Substitution = n∑i=1 (Izinga Lokushintsha I-Peak x NA) / 100
Imibandela yokwamukela: 6.2~6.9 ngezinga elimaphakathi lokushintsha
Ngayinye ye-betadex sulfobutyl ether sodium peaks I–X, bheka ububanzi bomkhawulo (% indawo ephakeme kakhulu) kuThebula 7.
Ithebula 7

• PH <791>: 4.0-6.8, kusixazululo esingu-30% (w/v) emanzini angenayo i-carbon dioxide
• UKUNIKEZWA KWAMANZI, Indlela I <921>: NMT 10.0%
IZIDINGO EZENGEZIWE
• UKUPAKASHWA KANYE NESIGCINI: Londoloza ezitsheni ezivalwe kahle, futhi ugcine endaweni eshisa kakhulu.Vikela kumswakama.
• UKULEBHULA: Ilebula ukukhombisa ukusetshenziswa kwayo lapho kwakhiwa amafomu omjovo.
• AMAZINGA EREferensi e-USP <11>
USP Beta Cyclodextrin RS
USP Betadex Sulfobutyl Ether Sodium RS
USP Endotoxin RS
I-USP Sodium Chloride RS■1S (NF30)