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

Betadex Sulfobutyl Ether Sodium
C42H70−nO35 · (C4H8SO3Na) n 2163 marka n = 6.5
Beta cyclodextrin sulfobutyl ethers, cusbada sodium;
Beta cyclodextrin sulfobutyl ether sodium [182410-00-0].
Qeexitaan
Betadex Sulfobutyl Ether Sodium waxaa lagu diyaariyaa alkylation of betadex iyadoo la isticmaalayo 1,4-butane sultone hoos yimaada xaaladaha aasaasiga ah.
Celceliska heerka beddelka ee betadex waa NLT 6.2 iyo NMT 6.9.
Waxay ka kooban tahay NLT 95.0% iyo NMT 105.0% ee C42H70−nO35 · (C4H8SO3Na) n (n = 6.2-6.9), oo lagu xisaabiyay ku salaysan anhydrous.
AQOONSIGA
• A. NUUXA NUUXDA AH <197K>
B. Wakhtiga haynta ee ugu sarraysa ee xal muunadku waxa ay u dhigantaa tan xalka caadiga ah, sida lagu helay Assay.
C. Waxay buuxisay shuruudaha imtixaanka celceliska heerka beddelka.
• D. Tijaabooyinka Aqoonsiga-GUUD, Sodium 〈191〉
ASSAY
HABKA
Marxaladda wareegta: 0.1 M Nitrate potassium oo isku jira acetonitrile iyo biyo (1:4)
Xalka caadiga ah: 10 mg/mL ee USP Betadex Sulfobutyl Ether Sodium RS ee wajiga mobaylka
Xalka muunada: 10 mg/mL ee Betadex Sulfobutyl Ether Sodium ee wajiga mobaylka
Nidaamka Chromatographic
(Fiiri Chromatography <621>, Habboonaanta Nidaamka.)
Habka: LC
Detector: Tilmaanta Refractive
Heerkulka baadhista: 35 ± 2°
Tiirka: 7.8-mm × 30-cm tiirka falanqaynta;xirxiran L37.[FIIRO GAAR AH-Ku luqluq tiirka xal acetonitrile iyo biyo ah (1:9) marka la dhammeeyo taxanaha orodka.]
Heerka socodka: 1.0 ml/min
Cabbirka duritaanka: 20 µL
Ku habboonaanta nidaamka .
Tusaale: Xalka caadiga ah
Shuruudaha ku habboonaanta
Qiyaasta heerka qaraabada: NMT 2.0%
Falanqaynta
Tusaalooyinka: Xalka caadiga ah iyo xalalka muunada
Xisaabi boqolkiiba betadex sulfobutyl ether sodium [C42H70−nO35 · (C4H8SO3Na)n] ee qaybta Betadex Sulfobutyl Ether Sodium ee la qaatay:
Natiijadu = (rU/rS) × (CS/CU) × 100
rU = jawaabta ugu sarreysa ee betadex sulfobutyl ether
soodhiyam ka xal muunad
rS = jawaabta ugu sarreysa ee betadex sulfobutyl ether
sodium ka xal Standard ah
CS = diiradda USP Betadex Sulfobutyl Ether
Sodium RS ee xalka caadiga ah (mg/mL)
CU = fiirsashada Betadex Sulfobutyl Ether Sodium ee xalka Muunada (mg/mL)
Shuruudaha aqbalaadda: 95.0% ~ 105.0% ku salaysan anhydrous
XANUUNKA
• Biraha culus, Habka II <231>: NMT 5 ppm
XADKA BETA CYCLODEXTRIN (BETADEX)
Xalka A: 25 mm sodium hydroxide
Xalka B: 250 mm sodium hydroxide iyo 1 M potassium nitrate
Marxaladda mobilada: Eeg shaxda 1.
Shaxda 1

Xalka caadiga ah: 2 µg/ml ee USP Beta Cyclodextrin RS
Tusaalaha xalalka: 2 mg/ml ee Betadex Sulfobutyl Ether Sodium
Nidaamka Chromatographic
(Fiiri Chromatography <621>, Habboonaanta Nidaamka iyo Ion Chromatography <1065>.)
Habka: IC
Baaraha: amperometry pulsed (unug amperometric ah oo leh koronto shaqaynaysa dahab iyo elektrode tixraac qalin ah)
Tiirka
Ilaaliyaha: 4.0-mm × 5-cm isweydaarsiga anion;xirxiran L61
Falanqaynta: 4.0-mm × 25-cm isweydaarsiga anion;
xirxiran L61
Heerkulka tiirka: 50 ± 2°
Heerka socodka: 1.0 ml/min
Cabbirka duritaanka: 20 µL
Waveform for pulsed amperometric detector: Eeg shaxda 2.
Shaxda 2

Ku habboonaanta nidaamka
Tusaale: Xalka caadiga ah
Shuruudaha ku habboonaanta
Qiyaasta heerka qaraabada: NMT 5.0%
Falanqaynta
Tusaalooyinka: Xalka caadiga ah iyo xalalka muunada
Xisaabi boqolkiiba beta cyclodextrin (betadex) ee qaybta Betadex Sulfobutyl Ether Sodium ee la qaatay:
Natiijadu = (rU/rS) × (CS/CU) × F × 100
rU = jawaabta ugu sarreysa ee beta cyclodextrin ee xalka Tusaalaha
rS = jawaabta ugu sarreysa ee beta cyclodextrin oo ka timid xalalka Standard
CS = U fiirsashada USP Beta Cyclodextrin RS ee xalka caadiga ah (µg/ml)
CU = fiirsashada Betadex Sulfobutyl Ether Sodium ee xalka Muunada (mg/mL)
F = qodobka beddelka (10-3 mg/µg)
Shuruudaha aqbalaadda: NMT 0.1%
XADKA 1,4-BUTANE SULTONE
Xalka caadiga ah ee gudaha: 0.25 µg/ml ee diethyl sulfone
Xalka saamiga caadiga ah A: 0.5 µg/ml ee 1,4-butane sultone
Xalka saamiga caadiga ah ee B: 1.0 µg/ml oo ah 1,4-butane sultone
Xalka saamiga caadiga ah C: 2.0 µg/ml oo ah 1,4-butane sultone
Tusaalaha xalalka saamiga: 250 mg/mL ee Betadex Sulfobutyl Ether Sodium ee xalka gudaha gudaha
Xalka madhan, iyo Tusaalaha xalalka A, B, C, iyo D:
Raac Jadwalka 3 si aad u dhigto tirada xalalka caadiga ah ee gudaha, xal kasta oo saamiga caadiga ah, saamiga saamiga, biyaha, ama chloride methylene ee tuubada tijaabada galaas kasta oo leh joogsi.[XUSUUS-Xidh-xidhan, 10-mL tuubbo tijaabo ah ayaa ku habboon.Ka soo saar wejiga organic ka mid ah fijaan GC oo shaabad.[FIIRO GAAR AH-Iyada oo taxaddar weyn leh u qaado qaddarka ugu yar ee suurtogalka ah ee wejiga aqueous.] Tirada lagu daray 1,4-butane sultone ee Tusaalaha xalalka A, B, C, iyo D waa 0.5, 1.0, 2.0, iyo 0 µg, siday u kala horreeyaan.
Shaxda 3

[FIIRO GAAR AH-Isdiyaari isla markiiba ka hor isticmaalka.]
Nidaamka Chromatographic
(Fiiri Chromatography <621>, Habboonaanta Nidaamka.)
Qaabka: GC
Baaraha: ionization ololka
Tiirka: 0.32-mm × 25-m tiirka xididka-silica ee isku dhafan;0.5-µm lakabka G46
Heerkulka
Baaraha: 270°
Dekadda durista: 200°
Tiirka: Eeg barnaamijka heerkulka shaxda 4
Shaxda 4
Heerkulka Hore (°) Heerkulka Sare (°/min) Heerkulka ugu dambeeya
100 10 200 -
200 35 270 5
Gaaska sidaha: Helium, sida caadiga ah 12 psi cadaadiska gudaha
Cabbirka duritaanka: 1.0 µL
Nooca duritaanka: Cirbad aan kala go'anayn 0.5 daqiiqo, ka dibna kala qaybsa 50 ml/daqiiqo.[FIIRO GAAR AH-Isticmaalka xadhkaha duritaanka ku habboon ee aan dillaacin ayaa lagula talinayaa.]
Ku habboonaanta nidaamka
Tusaale: Tusaalaha xalka B
[Xusuusin-Xilliyada haynta qaraabo ee diethyl sulfone iyo 1,4-butane sultone waa 0.7 iyo 1.0, siday u kala horreeyaan.]
Shuruudaha ku habboonaanta
Qiyaasta heerka qaraabada: NMT 10.0%
Falanqaynta
Tusaalooyinka: Xalka madhan, Tusaalaha xalalka A, B, C, iyo D
Sax saamiga jawaabaha ugu sarreeya ee 1,4-butane sultone ilaa diethyl sulfone ee Tusaalaha xalka A, B, C, ama D adoo kala jaraya saamiga jawaabaha ugu sarreeya ee 1,4-butane sultone ilaa ethyl sulfone ee xalka banaan .Qorshee saamiga la saxay ee jawaabta ugu sarreysa ee 1,4-butane sultone si jawaabta ugu sarreysa ee diethyl sulfone ku jirto Tusaalaha xalalka A, B, C ama D, marka loo eego tirada lagu daray, ee µg, ee 1,4-butane sultone.Ka saar xariiqda ku biirista dhibcaha garaafka ilaa uu ka buuxinayo dhidibka tirada.Fogaanta u dhaxaysa bartan iyo isgoyska faasasku waxay ka dhigan tahay tirada 1,4-butane sultone, A, ee µg, qaybta 4-mL ee saamiga saamiga saamiga.Xisaabi waxa ku jira 1,4-butane sultone ee qaybta Betadex Sulfobutyl Ether Sodium ee la qaatay:
Natiijadu = A/ (VExt × CU × F)
A = kor lagu go'aamiyay
VEXt = mugga saamiga saamiga saamiga ee loo adeegsaday tallaabada soo saarista, 4.0 mL
CU = fiirsashada Betadex Sulfobutyl Ether Sodium ee saamiga saamiga (mg/mL)
F = qodobka beddelka (10-3 g/mg)
Shuruudaha aqbalaadda: hydroxybutane-1-sulfonic acid, ama NMT 0.5 ppm
XUDUUDDA SODIUM Kloride, 4-HYDROXYBUTANE-1-SULFOIC ACIID, IYO BIS(4-SULFOBUTYL) Ether DISODIUM
Xalka A: 5 mM sodium hydroxide, degas weelka xiran ee 15 min
Xalka B: 25 mM sodium hydroxide, degas weelka xiran ee 15 min
Marxaladda mobilada: eeg Shaxda 5
Shaxda 5

Xalka dhaqidda tiirka A: 50 mM citrate sodium
Xalka dhaqidda tiirka B: 150 mm sodium hydroxide
Xalka caadiga ah: U diyaari xal adiga oo la og yahay 8 µg/mL ee USP Sodium Chloride RS, 4µg/mL ee 4-hydroxybutane-1-sulfonic acid, iyo 4 µg/mL oo bis (4-sulfobutyl) ether disodium.
Tusaalaha xalalka: 4 mg/ml ee Betadex Sulfobutyl Ether Sodium
Nidaamka Chromatographic
(Fiiri Chromatography <621>, Habboonaanta Nidaamka iyo Ion Chromatography <1065>.)
Habka: IC
Baaraha: Hab-dhaqanka
Qiyaasta: 30µS
Hadda: 100 mA
Tiirka: [Xusuusin-Dhammaadka orod kasta, nadiifi tiirka adigoo isticmaalaya xalinta tiirka A ee xadiga qulqulka 1 mL/min 35 min ka dibna isticmaal xalinta safafka B isla heerka socodka 35 min.]
Ilaalada: 4.0-mm × 5.0-cm isweydaarsiga anion;xirxiran L61
Falanqaynta: 4.0-mm × 25-cm isweydaarsiga anion;xirxiran L61
Heerkulka tiirka: 30°
Xakameeyaha: Micromembrane anion autosuppressor1 ama nidaamka xakamaynta kiimikada ku habboon
Xakamaynta: is-xakamaynta
Heerka socodka: 1.0 ml/min
Cabbirka duritaanka: 20 µL
Ku habboonaanta nidaamka
Tusaale: Xalka caadiga ah
[Xusuusin-Wakhtiyada haynta qaraabada waxa loo bixiyaa macluumaadka oo keliya.Wakhtiyada xajinta qaraabo ee 4-hydroxybutane-1-sulfonate ion, chloride ion, iyo bis(sulfobutyl) ether ion waa 1.0, 1.4, iyo 8.6, siday u kala horreeyaan.]
Shuruudaha ku habboonaanta
Xallinta: NLT 2.0
Qiyaasta heerka qaraabada: NMT 10.0%
Falanqaynta
Tusaalooyinka: Xalka caadiga ah iyo xalalka muunada
Xisaabi boqolkiiba sodium chloride, 4-hydroxybutane-1-sulfonic acid, ama bis(sulfobutyl) ether disodium ee qaybta Betadex Sulfobutyl Ether Sodium ee la qaatay:
Natiijadu = (rU/rS) × (CS/CU) × F × 100
rU = jawaabta ugu sarreysa ee sodium chloride, 4-hydroxybutane-1-sulfonic acid, ama bis (sulfobutyl) ether disodium oo ka yimid xal muunada
rS = jawaabta ugu sarreysa ee sodium chloride, 4-hydroxybutane-1-sulfonic acid, ama bis (sulfobutyl) ether disodium ee xalalka caadiga ah
CS = fiirsashada sodium chloride, 4-hydroxybutane-1-sulfonic acid, ama bis (sulfobutyl) ether disodium ee xalka caadiga ah (µg/ml)
CU = fiirsashada Betadex Sulfobutyl Ether Sodium ee xalka Muunada (mg/mL)
F = qodobka beddelka (10-3 0 100 0 mg/µg)
Shuruudaha aqbalaadda
Sodium chloride: NMT 0.2%
4-Hydroxybutane-1-sulfonic acid: NMT 0.09%
Bis(sulfobutyl) ether disodium: NMT 0.05%
IMTIXAANO GAAR AH
BACTERIAL ENDOTOXINS TEST <85>: Heerka bakteeriyada endotoxins waa sida shuruudaha hoos yimaada qaabka qiyaasta qiyaasta monograph(yada) ee Betadex Sulfobutyl Ether Sodium loo isticmaalo la buuxin karo.Halka calaamaddu ay sheegayso in Betadex Sulfobutyl Ether Sodium ay tahay in lagu sameeyo habayn dheeraad ah inta lagu jiro diyaarinta foomamka qiyaasta qiyaasta la isku duro, heerka endotoxins bakteeriyada waa sida shuruudaha hoos yimaada foomka qiyaasta ee monograph (s) kaas oo Betadex Sulfobutyl Ether Sodium loo isticmaalo waa lala kulmi karaa.
• Tijaabooyinka Tiro-koobka MICROBIAL <61> iyo IMTIXAANKA MIRROORGANISM-KA GAARKA AH <62>: Wadarta tirada microbial aerobic kama badna 100 cfu/g, wadarta guud ee caaryada iyo tirooyinka khamiirkuna kama badna 50 cfu/g.Waxay buuxinaysaa shuruudaha baaritaanka maqnaanshaha Escherichia coli.
Caddayn Xalka
Tusaalaha xalalka: 30% (w/v) xal
Falanqaynta: Baadh xalka muunada adiga oo isticmaalaya sanduuq khafiif ah oo ka soo horjeeda asalka caddaanka iyo madowga, oo qor joogitaanka wax kasta oo ceecaan ah, dhalaalid, fiyuusyo, xariijimo, ama arrimo kale oo shisheeye.
Shuruudaha aqbalaadda: Xalku waa cad yahay, oo asal ahaan ka madaxbannaan walxaha shisheeye.
• Celceliska Darajada Beddelka
Orod electrolyte: 30 mM benzoic acid oo lagu hagaajiyay pH ku haboon qalabka lagu daro 100 mM tris(hydroxymethyl) aminomethane buffer.
[FIIRO GAAR AH-Sababtoo ah kala duwanaanshaha u dhexeeya xididada, hal pH elektrolyte ah oo caalami ah lama cayimin.
Taa beddelkeeda, pH-ga ugu fiican ee la xidhiidha xidid kasta oo gaar ah waa in lagu go'aamiyaa sida uu qabo buug-gacmeedka.]
Xalka caadiga ah: 10 mg/mL oo ah USP Betadex Sulfobutyl Ether Sodium RS
Xalka muunada: 10 mg/ml ee Betadex Sulfobutyl Ether Sodium
Habka luqluqashada xididdada: Isticmaal fijaanno orod oo kala duwan si aad u biyo raaciso xididada iyo falanqaynta muunada.Samee biyo raacida hore ee falanqaynta maalin kasta ka hor falanqaynta kasta: ku raaci xididada 0.1 N sodium hydroxide 30 min, biyo NLT 2 h, iyo orodka elektrolytka ee NLT 1 h.Samee luqluqashada kahor duritaanka kahor duritaanka kasta sida soo socota.Ku raaci xididka xididka 0.1 N sodium hydroxide ee NLT 1 daqiiqo, iyo orodka elektrolytka NLT 3 daqiiqo.Haddii xidid cusub la isticmaalo, marka lagu daro luqluqashooyinka caadiga ah ee kor lagu sharaxay, xididka cusub wuxuu u baahan yahay biyo raacin ka hor isticmaalkiisa kowaad.Ku raaci xididka cusub ee 1 M sodium hydroxide 1 saac, oo ay ku xigto biyo raaci 2-saac ah.
Habka Electrophoretic
(Fiiri Capillary Electrophoresis <1053>.)
Qaabka: Waxqabadka sare ee CE
Detector: UV 200 nm rogan, oo leh xajmigiisu yahay 20nm.[Xusuusin-Mowjadaha ogaanshaha dhererka 205 nm oo leh xajmigiisu yahay 10 nm ayaa loo isticmaali karaa beddelka.]
Tiirka: Sodium Peaks I–X (% Meesha ugu sarreysa) 50-µm × 50-cm tiirka silica isku dhafan
Heerkulka tiirka: 25°
Korontada la dabaqay: 0.00 ilaa +30.00 kV toosan ka badan 10 daqiiqo, ka dibna 30 kV 20 daqiiqo oo kale
Cabbirka duritaanka: Mugga siman 0.5 psi ee 10 sekan
Ku habboonaanta nidaamka
Tusaale: Xalka caadiga ah
FIIRO GAAR AH- Fiiri jadwalka 6 qiyaasaha socdaalka qaraabada ee betadex sulfobutyl ether sodium peaks I–X ..., 10 beddelka sulfobutyl, siday u kala horreeyaan.Wakhtiyada socdaalka qaraabada waxa loogu talagalay ujeeddooyin macluumaad oo keliya si loo caawiyo aqoonsiga ugu sarreeya.]
Shaxda 6

Shuruudaha ku habboonaanta
Xallinta: NLT 0.9, inta u dhaxaysa betadex sulfobuty ether sodium peak IX iyo betadex sulfobutyl ether sodium peak X
Falanqaynta
Tusaalooyinka: Ku orod elektrolytka, biyaha, xalalka caadiga ah, iyo xal muunada
Ku duri xalalka caadiga ah iyo xalinta muunada adigoo isticmaalaya cadaadis kala duwan oo ah 0.5 psi, oo u dhiganta 34 mbar, 10 s, ka dibna lagu duro Run electrolyte at 0.5 psi ee 2 s.[FIIRO GAAR AH-Cadaadiska irbado waa in lagu sameeyaa fijaan biyo ah ama ku orod electrolyte meesha ugu dambaysa ee xididka.]
Diiwaangeli electropherograms, oo cabbir jawaabaha ugu sarreeya ee betadex sulfobutyl ether sodium peaks (I ilaa X).Xisaabi aagga ugu sarreeya ee la saxay, AI, mid kasta oo u sarreeya ee eletroferogram:
Meesha ugu sarreysa ee la saxay A = Meesha ugu sarreysa x Dhererka xididka waxtarka leh (cm) / Waqtiga socdaalka
Caadiye meelaha ugu sarreeya ee la saxay adiga oo mid walba u soo bandhigaya boqolkiiba wadarta guud ee baqshadda beddelka ee la saxay:
Aagga la magacaabay, NA: A / n∑i=1 Ai x 100
n = heerka ugu sarreeya ee beddelka
Go'aami celceliska heerka beddelka:
Celceliska Darajada Beddelka = n∑i=1 (Heerka Beddelka ugu sarreeya x NA) / 100
Shuruudaha aqbalaadda: 6.2 ~ 6.9 celceliska heerka beddelka
Mid kasta oo ka mid ah betadex sulfobutyl ether sodium ugu sarreysa I-X, eeg xadka xadka (% aagga ugu sarreeya) ee shaxda 7.
Shaxda 7

PH <791>: 4.0-6.8, ku jira 30% (w/v) xal biyo la'aan ah
• Go'aaminta biyaha, Habka I <921>: NMT 10.0%
SHURUUD DHEERAAD AH
Baakadaha iyo Kaydinta: Ku kaydi weelasha si fiican u xidhan, kuna kaydi heerkulka qolka.Ka ilaali qoyaanka.
Calaamadaynta: Calaamadee si aad u muujiso isticmaalkeeda marka la samaynayo foomamka qiyaasta qiyaasta la isku duro.
• HEERARKA Tixraaca USP <11>
USP Beta Cyclodextrin RS
USP Betadex Sulfobutyl Ether Sodium RS
USP Endotoxin RS
USP Sodium Chloride RS■1S (NF30)