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

Betadex Sulfobutyl Etere Sodium
C42H70−nO35 · (C4H8SO3Na)n 2163 xa n = 6.5
I-Beta cyclodextrin sulfobutyl ethers, iityuwa zesodium;
I-Beta cyclodextrin sulfobutyl ether sodium [182410-00-0].
INGCACISO
I-Betadex Sulfobutyl Ether Sodium ilungiswe yi-alkylation ye-betadex usebenzisa i-1,4-butane sultone phantsi kweemeko ezisisiseko.
Umndilili weqondo lotshintsho kwi-betadex yi-NLT 6.2 kunye ne-NMT 6.9.
Iqulethe i-NLT 95.0% kunye ne-NMT 105.0% ye-C42H70−nO35 · (C4H8SO3Na)n (n = 6.2–6.9), ibalwa ngokwesiseko se-anhydrous.
UKUCHAZA
• A. UKUFUNWA KWE-IFRARED <197K>
• B. Ixesha lokugcinwa kwencopho enkulu yeSampuli yesisombululo ihambelana nesisombululo esisemgangathweni, njengoko sifunyenwe kwi-Assay.
• C. Iyazifezekisa iimfuno zovavanyo lwe-Average Degree of Substitution.
• D. IIMVAVANYO ZOKUCHAZA NGOKUBANZI, iSodium 〈191〉
UVAVANYO
• INKQUBO
Isigaba seselula: 0.1 M potassium nitrate kumxube we-acetonitrile kunye namanzi (1: 4)
Isisombululo esisemgangathweni: 10 mg / mL ye-USP Betadex Sulfobutyl Ether Sodium RS kwisigaba seMobile
Isisombululo sesampuli: 10 mg / mL ye-Betadex Sulfobutyl Ether Sodium kwisigaba seMobile
Inkqubo yeChromatographic
(Jonga iChromatography <621>, Ukufaneleka kweNkqubo.)
Indlela: LC
Umtshina: Isalathiso sokuqhafaza
Ubushushu be-detector: 35 ± 2 °
Ikholomu: 7.8-mm × 30-cm ikholamu yokuhlalutya;ukupakisha i-L37.[QAPHELA-Hlala ikholamu ngesisombululo se-acetonitrile kunye namanzi (1: 9) ekugqityweni koluhlu lokuqhuba.]
Izinga lokuhamba: 1.0 mL / min
Ubungakanani betofu: 20 µL
Ukufaneleka kwenkqubo .
Isampulu: Isisombululo esisemgangathweni
Iimfuno zokufaneleka
Ukutenxa komgangatho ozalanayo: NMT 2.0%
Uhlalutyo
Iisampulu: Isisombululo esisemgangathweni kunye nesisombululo seSampuli
Bala ipesenti ye-betadex sulfobutyl ether sodium [C42H70−nO35 · (C4H8SO3Na)n] kwisahlulo seBetadex Sulfobutyl Ether Sodium ethathiweyo:
Isiphumo = (rU/rS) × (CS/CU) × 100
rU = impendulo ephezulu ye-betadex sulfobutyl ether
sodium evela kwiSampuli isisombululo
rS = impendulo ephezulu ye-betadex sulfobutyl ether
sodium ukusuka kwisisombululo esiPhakathi
CS = ukuxinwa kwe-USP Betadex Sulfobutyl Ether
Isodium RS kuMgangatho wesisombululo (mg/mL)
I-CU = i-concentration ye-Betadex Sulfobutyl Ether Sodium kwi-Sample solution (mg / mL)
Indlela yokwamkela: 95.0% ~ 105.0% kwisiseko se-anhydrous
UBUNGCOLA
• IIMETALI EZINZIMA, Indlela II <231>: NMT 5 ppm
• UMDA WE-BETA CYCLODEXTRIN (BETADEX)
Isisombululo A: 25 mM sodium hydroxide
Isisombululo B: 250 mM sodium hydroxide kunye ne-1 M potassium nitrate
Isigaba esiphathwayo: Jonga iTheyibhile 1.
Uluhlu loku-1

Isisombululo esisemgangathweni: 2 µg/mL ye-USP Beta Cyclodextrin RS
Isisombululo sesampuli: 2 mg / mL ye-Betadex Sulfobutyl Ether Sodium
Inkqubo yeChromatographic
(Jonga i-Chromatography <621>, Ukufaneleka kweNkqubo kunye ne-Ion Chromatography <1065>.)
Indlela: IC
Umtshina: I-amperometry ephuhlisiweyo (iseli ye-amperometric ene-electrode esebenzayo yegolide kunye ne-electrode yereferensi yesilivere)
Umqolo
Umlindi: 4.0-mm × 5-cm anion-exchange;ukupakisha i-L61
Uhlalutyo: 4.0-mm × 25-cm anion-exchange;
ukupakisha i-L61
Ubushushu bekholamu: 50 ± 2 °
Izinga lokuhamba: 1.0 mL / min
Ubungakanani betofu: 20 µL
I-Waveform ye-pulsed amperometric detector: Jonga iTheyibhile yesi-2.
Uluhlu lwesi-2

Ukufaneleka kwenkqubo
Isampulu: Isisombululo esisemgangathweni
Iimfuno zokufaneleka
Ukutenxa umgangatho ozalanayo: NMT 5.0%
Uhlalutyo
Iisampulu: Isisombululo esisemgangathweni kunye nesisombululo seSampuli
Bala ipesenti ye-beta cyclodextrin (betadex) kwinxalenye yeBetadex Sulfobutyl Ether Sodium ethathiweyo:
Isiphumo = (rU/rS) × (CS/CU) × F × 100
rU = impendulo ephezulu ye-beta cyclodextrin kwisisombululo seSampuli
rS = impendulo ephezulu ye-beta cyclodextrin ukusuka kwisisombululo esiPhakathi
CS = ukuxinwa kwe-USP Beta Cyclodextrin RS kwisisombululo esiPhakathi (µg/mL)
I-CU = i-concentration ye-Betadex Sulfobutyl Ether Sodium kwi-Sample solution (mg / mL)
F = into yokuguqula (10-3 mg/µg)
Indlela yokwamkelwa: NMT 0.1%
• UMDA WE-1,4-BUTANE SULTONE
Isisombululo somgangatho wangaphakathi: 0.25 µg/mL ye-diethyl sulfone
Isisombululo sesitokhwe esisemgangathweni A: 0.5 µg/mL ye-1,4-butane sultone
Isisombululo sesitokhwe esisemgangathweni B: 1.0 µg/mL ye-1,4-butane sultone
Isisombululo sesitokhwe esisemgangathweni C: 2.0 µg/mL ye-1,4-butane sultone
Isisombululo sesitokhwe sesampuli: 250 mg / mL yeBetadex Sulfobutyl Ether Sodium kwisisombululo esisemgangathweni sangaphakathi
Isisombululo esingenanto, kunye nezisombululo zeSampuli A, B, C, kunye no-D:
Landela iThebhile 3 ukubeka ubuninzi besisombululo somgangatho wangaphakathi, isisombululo ngasinye sesitokhwe esisemgangathweni, isisombululo sesitokhwe seSampule, amanzi, okanye i-methylene chloride kwityhubhu yovavanyo lweglasi nganye ene-stopper.[QAPHELA-I-screw-capped, ityhubhu yokuvavanya i-10-mL ifanelekile.] Hlanganisa kwi-vortex mixer ityhubhu nganye yokuvavanya i-30 s, kwaye uvumele ukuba ime ubuncinane imizuzu emi-5 okanye kude kube nokuhlukana okupheleleyo kwesigaba.Khipha isigaba se-organic kwi-vial ye-GC kunye netywina.[QAPHELA-Ngononophelo olukhulu thatha ubuncinci obunokwenzeka besigaba se-aqueous.] Izixa ezongeziweyo ze-1,4-butane sultone kwi-Sample solutions A, B, C, and D are 0.5, 1.0, 2.0, and 0 µg, ngokulandelanayo.
Itheyibhile 3

[QAPHELA-Lungisa ngokukhawuleza phambi kokusetyenziswa.]
Inkqubo yeChromatographic
(Jonga iChromatography <621>, Ukufaneleka kweNkqubo.)
Indlela: GC
Umtshina: Iionization yomlilo
Ikholamu: 0.32-mm × 25-m fused-silica ikholamu capillary;0.5-µm umaleko wesigaba G46
Ubushushu
Umtshina: 270 °
I-port yokutofa: 200 °
Uluhlu: Bona inkqubo yobushushu kwiTheyibhile 4
Uluhlu lwesi-4
Iqondo lobushushu lokuqala (°) Irempu yoBubushushu (°/min) Iqondo lobushushu lokuGqibela (°) Ukubamba ixesha kuBubushushu bokugqibela (umzuzu)
100 10 200 -
200 35 270 5
Irhasi yeCarrier: Helium, ngokuqhelekileyo kwi-12 psi inlet yoxinzelelo
Ubungakanani bokutofa: 1.0 µL
Uhlobo lwe-injection: I-injection ye-splitless ye-0.5 min, ize yahlulwe kwi-50 mL / min.[QAPHELA-Ukusetyenziswa kwesitofu esifanelekileyo esingacalulwanga kuyacetyiswa.]
Ukufaneleka kwenkqubo
Isampulu: Isampuli yesisombululo B
[QAPHELA-Amaxesha anxulumeneyo okugcina i-diethyl sulfone kunye ne-1,4-butane sultone yi-0.7 kunye ne-1.0, ngokulandelelanayo.]
Iimfuno zokufaneleka
Ukutenxa umgangatho ozalanayo: NMT 10.0%
Uhlalutyo
Iisampulu: Isisombululo esingenanto, izisombululo zesampulu A, B, C, kunye noD
Lungisa umlinganiselo weempendulo eziphezulu ze-1,4-butane sultone kwi-diethyl sulfone kwiSampuli isisombululo A, B, C, okanye D ngokukhupha umlinganiselo weempendulo eziphezulu ze-1,4-butane sultone kwi-ethyl sulfone kwisisombululo esingenanto. .Cwangcisa umlinganiselo ochanekileyo wepeak impendulo ye-1,4-butane sultone ukuya kwincopho yempendulo ye-diethyl sulfone kwiSampule yesisombululo A, B, C okanye D, xa kuthelekiswa nobuninzi obudityanisiweyo, kwi-µg, ye-1,4-butane sultone.Yongeza umgca odibanisa amanqaku kwigrafu de udibane ne-axis yobungakanani.Umgama phakathi kwale ndawo kunye nokuhlangana kwee-axes umele ubuninzi be-1,4-butane sultone, A, kwiµg, kwisahlulo se-4-mL seSampule yesisombululo sesitokhwe.Bala umxholo we-1,4-butane sultone kwisahlulo se-Betadex Sulfobutyl Ether Sodium ethathiweyo:
Isiphumo = A/(VExt × CU × F)
A = imiselwe ngasentla
I-VExt = umthamo weSampuli yesisombululo sesitokhwe esisetyenziswe kwisinyathelo sokukhutshwa, i-4.0 mL
I-CU = i-concentration ye-Betadex Sulfobutyl Ether Sodium kwi-Sample stock solution (mg / mL)
F = into yokuguqula (10-3 g/mg)
Indlela yokwamkela: i-hydroxybutane-1-sulfonic acid, okanye i-NMT 0.5 ppm
• UMDA WESODIUM CHLORIDE, 4-HYDROXYBUTANE-1-SULFONIC ACID, KUNYE NE-BIS(4-SULFOBUTYL) ETHI I-DISODIUM
Isisombululo A: I-5 mM i-sodium hydroxide, i-degas kwisitya esivaliweyo se-15 min
Isisombululo B: I-25 mM i-sodium hydroxide, i-degas kwisitya esivaliweyo se-15 min
Isigaba esiphathwayo: Jonga iTheyibhile 5
Uluhlu 5

Isisombululo sokuhlamba ikholomu A: 50 mM sodium citrate
Isisombululo sokuhlamba ikholomu B: 150 mM sodium hydroxide
Isisombululo esisemgangathweni: Lungiselela isisombululo esinogxininiso olwaziwayo lwe-8 µg/mL ye-USP ye-Sodium Chloride RS, i-4µg/mL ye-4-hydroxybutane-1-sulfonic acid, kunye ne-4 µg/mL ye-bis (4-sulfobutyl) ether disodium.
Isisombululo sesampuli: 4 mg / mL ye-Betadex Sulfobutyl Ether Sodium
Inkqubo yeChromatographic
(Jonga i-Chromatography <621>, Ukufaneleka kweNkqubo kunye ne-Ion Chromatography <1065>.)
Indlela: IC
Umtshina: Ukuqhuba
Uluhlu: 30 µS
Okwangoku: 100 mA
Ikholomu: [QAPHELA-Ekupheleni kokubaleka ngalunye, coca ikholamu usebenzisa isisombululo sokuhlamba iKholamu A ngesantya sokuhamba kwe-1 mL/min ye-35 min emva koko usebenzisa iKholamu yokuhlamba isisombululo B kwisantya esifanayo sokuhamba kwe-35 min.]
Umlindi: 4.0-mm × 5.0-cm anion-exchange;ukupakisha i-L61
Uhlalutyo: 4.0-mm × 25-cm anion-exchange;ukupakisha i-L61
Ubushushu bekholamu: 30 °
Umcinezeli: I-Micromembrane anion autosuppressor1 okanye inkqubo efanelekileyo yokunciphisa imichiza
Ukucinezela: Ukunyanzeliswa ngokuzenzekelayo
Izinga lokuhamba: 1.0 mL / min
Ubungakanani betofu: 20 µL
Ukufaneleka kwenkqubo
Isampulu: Isisombululo esisemgangathweni
[QAPHELA-Amaxesha okugcina anxulumeneyo anikezelwe ngolwazi kuphela.Amaxesha okugcina anxulumene ne-4-hydroxybutane-1-sulfonate ion, ion chloride, kunye ne-bis(sulfobutyl) ether ion yi-1.0, 1.4, kunye ne-8.6, ngokulandelanayo.]
Iimfuno zokufaneleka
Isisombululo: NLT 2.0
Ukutenxa umgangatho ozalanayo: NMT 10.0%
Uhlalutyo
Iisampulu: Isisombululo esisemgangathweni kunye nesisombululo seSampuli
Bala ipesenti ye-sodium chloride, i-4-hydroxybutane-1-sulfonic acid, okanye i-bis (sulfobutyl) i-ether disodium kwisahlulo se-Betadex Sulfobutyl Ether Sodium ethathiweyo:
Isiphumo = (rU/rS) × (CS/CU) × F × 100
i-rU = impendulo ephezulu ye-sodium chloride, i-4-hydroxybutane-1-sulfonic acid, okanye i-bis (sulfobutyl) i-ether disodium evela kwiSample isisombululo
rS = impendulo ephezulu ye-sodium chloride, i-4-hydroxybutane-1-sulfonic acid, okanye i-bis (sulfobutyl) i-ether disodium evela kwisisombululo esiPhakathi
I-CS = i-concentration ye-sodium chloride, i-4-hydroxybutane-1-sulfonic acid, okanye i-bis (sulfobutyl) i-ether disodium kwisisombululo soMgangatho (µg / mL)
I-CU = i-concentration ye-Betadex Sulfobutyl Ether Sodium kwi-Sample solution (mg / mL)
F = into yokuguqula (10−3 0 100 0 mg/µg)
Iinqobo zokwamkelwa
Isodium chloride: NMT 0.2%
4-Hydroxybutane-1-sulfonic acid: NMT 0.09%
I-Bis(sulfobutyl) ether disodium: NMT 0.05%
IIMVAVANYO EZITHILE
UVAVANYO lwe-ENDOTOXINS YE-BACTERIAL <85>: Inqanaba leendotoxins zebhaktheriya linjalo ukuba imfuno phantsi kwefom ye-dosage echaphazelekayo i-monograph (s) apho i-Betadex Sulfobutyl Ether Sodium isetyenziselwa khona.Apho ilebula ichaza ukuba i-Betadex Sulfobutyl Ether Sodium kufuneka ixhomekeke ekuqhubekeni phambili ngexesha lokulungiswa kweefom ze-dosage ye-injection, inqanaba le-endotoxins yebhaktheriya kukuba imfuno phantsi kwefom ye-dosage efanelekileyo i-monograph (s) apho i-Betadex Sulfobutyl Ether Sodium isetyenziswa. inokuhlangatyezwana nayo.
• UVAVANYO LWEMICROBIAL ENUMERATION <61> kunye noVAVANYO LWEMICROORGANISMS ESHICILEYO <62>: Itotali ye-aerobic microbial count ayigqithi kwi-100 cfu/g, kwaye inani elidityanisiweyo lokungunda kunye negwele alidluli kwi-50 cfu/g.Ihlangabezana neemfuno zovavanyo lokungabikho kwe-Escherichia coli.
• UKUCACA NGESONDLULO
Isisombululo sesampuli: 30% (w/v) isisombululo
Uhlalutyo: Phonononga isisombululo seSampuli usebenzisa ibhokisi yokukhanya ngokuchasene nemvelaphi emhlophe nemnyama, kwaye urekhode ubukho bayo nayiphi na inkungu, i-fluorescence, iifayibha, amachaphaza, okanye enye into yangaphandle.
Iinqobo zokwamkelwa: Isisombululo sicacile, kwaye ngokusisiseko sikhululekile kumasuntswana omcimbi wangaphandle.
• I-Avareji yedigri yokutshintshwa
Qhuba i-electrolyte: 30 mM benzoic acid kwaye ilungelelaniswe kwi-pH elungele isixhobo esisetyenziswe ngokudityaniswa kwe-100 mM tris(hydroxymethyl) aminomethane buffer.
[QAPHELA-Ngenxa yokwahluka phakathi kwee-capillaries, i-electrolyte enye esebenza kwihlabathi jikelele pH ayichazwanga.
Endaweni yoko, eyona pH edityaniswe necapillary nganye kufuneka imiselwe ngokwesixhobo sokufundisa.]
Isisombululo esisemgangathweni: 10 mg / mL ye-USP Betadex Sulfobutyl Ether Sodium RS
Isisombululo sesampuli: 10 mg / mL ye-Betadex Sulfobutyl Ether Sodium
Inkqubo yokuhlanjululwa kweCapillary: Sebenzisa iibhotile ze-electrolyte eziqhutywa ngokwahlukeneyo zokuhlanjululwa kwe-capillary kunye nohlalutyo lwesampulu.Yenza ukuhlalutya kwangaphambili ukuhlalutya imihla ngemihla ngaphambi kokuhlalutya ngalunye: hlambulula i-capillary nge-0.1 N sodium hydroxide kwi-30 min, ngamanzi e-NLT 2 h, kunye ne-Run electrolyte ye-NLT 1 h.Yenza i-rinses pre-injection phambi kwenaliti nganye ngolu hlobo lulandelayo.Hlanza i-capillary nge-0.1 N sodium hydroxide ye-NLT 1 min, kunye ne-Run electrolyte ye-NLT 3 min.Ukuba i-capillary entsha isetyenzisiweyo, ngaphezu kweerinses eziqhelekileyo ezichazwe ngasentla, i-capillary entsha idinga ukuhlanjululwa ngaphambi kokusetyenziswa kwayo kokuqala.Hlanza i-capillary entsha nge-1 M ye-sodium hydroxide kwi-1 h, ilandelwe yi-2-h yokuhlanjululwa kwamanzi.
Inkqubo ye-Electrophoretic
(Jonga iCapillary Electrophoresis <1053>.)
Imowudi: Ukusebenza okuphezulu kweCE
I-Detector: I-Inverse UV 200 nm, kunye ne-bandwidth ye-20nm.[QAPHELA-Ubude bobude be-205 nm kunye ne-bandwidth ye-10nm ingasetyenziswa njengenye indlela.]
Ikholamu: IiNcopho zeSodium I–X (% Indawo eNcopho) 50-µm × 50-cm ikholamu yesilica edityanisiweyo
Ubushushu bekholamu: 25 °
Umbane osetyenziswayo: 0.00 ukuya +30.00 kV umgca werempu ngaphezulu kwe-10 min, emva koko ube yi-30 kV enye imizuzu engama-20
Ubungakanani be-injection: Imiqulu elinganayo kwi-0.5 psi kwi-10 s
Ukufaneleka kwenkqubo
Isampulu: Isisombululo esisemgangathweni
[QAPHELA-Jonga iThebhile 6 malunga namaxesha asondeleneyo okufuduka kwe-betadex sulfobutyl ether sodium peaks I-X (betadex sulfobutyl ether sodium peaks I, II, III, ..., X, iqulethe i-molecule ye-beta cyclodextrin ene-1, 2, 3, ..., 10 sulfobutyl substituent(s), ngokulandelelanayo).Amaxesha okufuduka ahambelanayo ngawenjongo yolwazi kuphela ukunceda ekuchongweni kwencopho.]
Uluhlu 6

Iimfuno zokufaneleka
Isisombululo: NLT 0.9, phakathi kwe-betadex sulfobuty ether sodium peak IX kunye ne-betadex sulfobutyl ether yesodium peak X
Uhlalutyo
Iisampulu: Sebenzisa i-electrolyte, amanzi, isisombululo esiPhakathi, kunye nesisombululo seSampuli
Ijova isisombululo soMgangatho kunye nesisombululo seSampuli ngokusebenzisa uxinzelelo oluhlukeneyo lwe-0.5 psi, elilingana ne-34 mbar, kwi-10 s, ilandelwa yi-injection ye-Run electrolyte kwi-0.5 psi kwi-2 s.[QAPHELA-Inaliti zoxinzelelo kufuneka zenziwe ngevial ​​yamanzi okanye Qalisa i-electrolyte ekupheleni kwecapillary.]
Rekhoda i-electropherograms, kwaye ulinganise iimpendulo eziphezulu ze-betadex sulfobutyl ether sodium peaks (I ukuya ku-X).Bala indawo eyincopho echanekileyo, i-AI, kwincopho nganye kwi-eletropherogram:
Indawo eNcopho eLungileyo A = Indawo eNcopho x Ubude beCapillary obusebenzayo (cm) / Ixesha lokufuduka
Lungiselela iindawo ezizincopho ezilungisiweyo ngokubonisa nganye njengepesenti yommandla wemvulophu ochanekileyo olungisiweyo:
Ummandla oNomaza, NA: A / n∑i=1 Ai x 100
n = inqanaba eliphezulu lokutshintsha
Qinisekisa iqondo eliphakathi lokutshintsha:
I-Avareji yesiDanga soTshintsho = n∑i=1 (Inqanaba lokuTshintshwa kweNcopho x NA) / 100
Iikhrayitheriya zokwamkelwa: 6.2 ~ 6.9 kwiqondo eliphakathi lokutshintshwa
Ngomnye we-betadex sulfobutyl ether sodium peaks I-X, jonga umda womda (% indawo ephezulu) kwiThebhile 7.
Uluhlu 7

• PH <791>: 4.0-6.8, kwisisombululo se-30% (w/v) kwi-carbon dioxide-free water
• UKUMISELWA KWAMANZI, Indlela I <921>: NMT 10.0%
IIMFUNO EZONGEZELELWEYO
• UKUPAKISHWA NOKUGCINA: Zigcine kwizikhongozeli ezivaliweyo, uze uzigcine kwindawo yobushushu begumbi.Khusela ukufuma.
• UKULEBHULA: Ileyibhelishe ukubonisa ukusetyenziswa kwayo xa kusenziwa iifomu zethamo elitofwayo.
• IMIGANGATHO YE-USP REFERENCE <11>
USP Beta Cyclodextrin RS
USP Betadex Sulfobutyl Etere Sodium RS
USP Endotoxin RS
USP Sodium Chloride RS■1S (NF30)