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

Betadex Sulfobutyl Ether Sodium
C42H70−nO35 · (C4H8SO3Na)n 2163 apo n = 6.5
Beta cyclodextrin sulfobutyl ethers, sodium munyu;
Beta cyclodextrin sulfobutyl ether sodium [182410-00-0].
DEFINITION
Betadex Sulfobutyl Ether Sodium inogadzirwa nealkylation ye betadex uchishandisa 1,4-butane sultone pasi pemamiriro ekutanga.
Avhareji yedhigirii yekutsiva mubetadex iNLT 6.2 uye NMT 6.9.
Iine NLT 95.0% uye NMT 105.0% yeC42H70−nO35 · (C4H8SO3Na)n (n = 6.2–6.9), yakaverengwa pane anhydrous basis.
KUZIVA
• A. INFRARED ABSORPTION <197K>
• B. Nguva yekuchengeta yenhongonya huru yeSample solution inoenderana neiyo yestandard solution, sezvakawanikwa muAssay.
• C. Inosangana nezvinodiwa zvekuedzwa kweAverage Degree of Substitution.
• D. ZVIYEDZO ZVOKUZIVA-ZVINHU, Sodium 〈191〉
ASSAY
• MAITIRO
Nharembozha: 0.1 M potassium nitrate mumusanganiswa weacetonitrile nemvura (1: 4)
Standard solution: 10 mg/mL yeUSP Betadex Sulfobutyl Eteri Sodium RS muMobile phase
Sample solution: 10 mg/mL yeBetadex Sulfobutyl Ether Sodium muMobile phase
Chromatographic system
(Ona Chromatography <621>, System Suitability.)
Modhi: LC
Detector: Refractive index
Detector tembiricha: 35 ± 2 °
Column: 7.8-mm × 30-cm analytical column;kurongedza L37.[Cherechedza-Simbura mbiru nemhinduro yeacetonitrile nemvura (1:9) pakupedzwa kwekumhanya kwenhevedzano.]
Kuyerera kweyero: 1.0 mL/min
Jekiseni saizi: 20 µL
Kukodzera kwehurongwa .
Muenzaniso: Standard solution
Kukodzera zvinodiwa
Kutsauswa muyero: NMT 2.0%
Analysis
Samples: Yakajairwa mhinduro uye Sample mhinduro
Verenga chikamu chebetadex sulfobutyl ether sodium [C42H70−nO35 · (C4H8SO3Na)n] muchikamu cheBetadex Sulfobutyl Ether Sodium yakatorwa:
Mhedzisiro = (rU/rS) × (CS/CU) × 100
rU = peak mhinduro ye betadex sulfobutyl ether
sodium kubva Sample solution
rS = mhinduro yepamusoro ye betadex sulfobutyl ether
sodium kubva kune Standard solution
CS = kusangana kweUSP Betadex Sulfobutyl Ether
Sodium RS muiyo Standard mhinduro (mg/mL)
CU = kusangana kweBetadex Sulfobutyl Ether Sodium muSample solution (mg/mL)
Maitiro ekugamuchira: 95.0% ~ 105.0% pane anhydrous basis
KUSIRIRA
• METARI ZVIKURU, Nzira II <231>: NMT 5 ppm
• LIMIT OF BETA CYCLODEXTRIN (BETADEX)
Mhinduro A: 25 mM sodium hydroxide
Mhinduro B: 250 mM sodium hydroxide uye 1 M potassium nitrate
Nharembozha: Ona Tafura 1.
Tafura 1

Mushonga wakajairika: 2 µg/mL yeUSP Beta Cyclodextrin RS
Sample solution: 2 mg/mL yeBetadex Sulfobutyl Ether Sodium
Chromatographic system
(Ona Chromatography <621>, System Suitability uye Ion Chromatography <1065>.)
Modhi: IC
Detector: Pulsed amperometry (amperometric cell ine goridhe inoshanda electrode uye sirivheri referensi electrode)
Column
Guard: 4.0-mm × 5-cm anion-exchange;kurongedza L61
Analytical: 4.0-mm × 25-cm anion-exchange;
kurongedza L61
Column tembiricha: 50 ± 2 °
Kuyerera kweyero: 1.0 mL/min
Jekiseni saizi: 20 µL
Waveform ye pulsed amperometric detector: Ona Tafura 2.
Tafura 2

Kukodzera kwehurongwa
Muenzaniso: Standard solution
Kukodzera zvinodiwa
Kutsauswa kwechiyero: NMT 5.0%
Analysis
Samples: Yakajairwa mhinduro uye Sample mhinduro
Verenga chikamu che beta cyclodextrin (betadex) muchikamu cheBetadex Sulfobutyl Ether Sodium yakatorwa:
Mhedzisiro = (rU/rS) × (CS/CU) × F × 100
rU = peak mhinduro ye beta cyclodextrin kubva kuSample solution
rS = peak mhinduro ye beta cyclodextrin kubva kune Standard solution
CS = kusungwa kweUSP Beta Cyclodextrin RS muStandard solution (µg/mL)
CU = kusangana kweBetadex Sulfobutyl Ether Sodium muSample solution (mg/mL)
F = shanduko chinhu (10-3 mg/µg)
Maitiro ekugamuchira: NMT 0.1%
• LIMIT OF 1,4-BUTANE SULTONE
Yemukati mwero mhinduro: 0.25 µg/mL ye diethyl sulfone
Standard stock solution A: 0.5 µg/mL ye1,4-butane sultone
Standard stock solution B: 1.0 µg/mL ye1,4-butane sultone
Standard stock solution C: 2.0 µg/mL ye1,4-butane sultone
Sample stock solution: 250 mg/mL yeBetadex Sulfobutyl Ether Sodium muInternal standard solution
Mhinduro isina chinhu, uye Sample mhinduro A, B, C, uye D:
Tevedzera Tafura 3 kuti uise huwandu hweYemukati mwero mhinduro, yega yega Standard stock solution, Sample stock solution, mvura, kana methylene chloride mune yega yega girazi chubhu yekuyedza ine chimiso.[Cherechedza-A screw-capped, 10-mL test chubhu yakakodzera.] Sanganisa pane vortex mixer yega yega test chubhu ye30 s, uye uibvumire kumira kweinenge 5 min kana kusvika kupatsanurwa kwakakwana kwechikamu.Bvisa iyo organic chikamu muGC vial uye chisimbiso.[Cherechedza-Nekuchenjerera kukuru tora hushoma hunobvira huwandu hwechikamu chemvura.] Yakawedzerwa huwandu hwe1,4-butane sultone muSample solutions A, B, C, uye D ndeye 0.5, 1.0, 2.0, uye 0 µg, zvichiteerana.
Tafura 3

[Cherechedza-Gadzirira pakarepo usati washandisa.]
Chromatographic system
(Ona Chromatography <621>, System Suitability.)
Modhi: GC
Detector: Moto ionization
Column: 0.32-mm × 25-m fused-silica capillary column;0.5-µm musara wechikamu G46
Tembiricha
Detector: 270 °
Injection port: 200 °
Column: Ona chirongwa chekushisa muTafura 4
Tafura 4
Initial Temperature (°) Temperature Ramp (°/min) Yekupedzisira Tembiricha (°) Bata Nguva paFinal Temperature (min)
100 10 200 -
200 35 270 5
Inotakura gasi: Helium, kazhinji pa12 psi inlet pressure
Jekiseni saizi: 1.0 µL
Jekiseni rudzi: Splitless jekiseni re 0.5 min, wobva wapatsanurwa pa50 mL/min.[Cherechedza-Kushandiswa kwejekiseni rejekiseni rakapatsanuka kunokurudzirwa.]
Kukodzera kwehurongwa
Muenzaniso: Mhinduro yemuenzaniso B
[Cherechedza-Nguva dzekuchengeta diethyl sulfone uye 1,4-butane sultone i0.7 uye 1.0, zvichiteerana.]
Kukodzera zvinodiwa
Kutsauswa kwechiyereko: NMT 10.0%
Analysis
Samples: mhinduro isina chinhu, Sample mhinduro A, B, C, uye D
Gadzirisa reshiyo yepeak mhinduro dze1,4-butane sultone kune diethyl sulfone muSample solution A, B, C, kana D nekubvisa reshiyo yepeak mhinduro dze1,4-butane sultone kune ethyl sulfone muBlank solution. .Ronga reshiyo yakagadziriswa yepeak response ye1,4-butane sultone kusvika peak response yediethyl sulfone muSample solution A, B, C kana D, maringe neuwandu hwakawedzerwa, muµg, hwe1,4-butane sultone.Wedzera mutsara uchibatanidza mapoinzi pagirafu kusvika wasangana nehuwandu hweakisi.Chinhambwe chiri pakati peiyi poindi uye pamharadzano yematemo chinomiririra huwandu hwe1,4-butane sultone, A, muµg, muchikamu che4-mL cheSample stock solution.Verenga zviri mukati me1,4-butane sultone muchikamu cheBetadex Sulfobutyl Ether Sodium yakatorwa:
Mhedzisiro = A/(VExt × CU × F)
A = yakatarwa pamusoro
VExt = vhoriyamu yeSample stock solution inoshandiswa mudanho rekubvisa, 4.0 mL
CU = kusangana kweBetadex Sulfobutyl Ether Sodium muSample stock solution (mg/mL)
F = shanduko chinhu (10-3 g/mg)
Maitiro ekugamuchira: hydroxybutane-1-sulfonic acid, kana NMT 0.5 ppm
• LIMIT YESODIUM CHLORIDE, 4-HYDROXYBUTANE-1-SULFONIC ACID, UYE BIS(4-SULFOBUTYL) ETHER DISODIUM
Mhinduro A: 5 mM sodium hydroxide, degas mumudziyo wakavharwa we15 min
Mhinduro B: 25 mM sodium hydroxide, degas mumudziyo wakavharwa we15 min
Nharembozha: Ona Tafura 5
Tafura 5

Column wash solution A: 50 mM sodium citrate
Column wash solution B: 150 mM sodium hydroxide
Mushonga wakajairwa: Gadzirira mhinduro ine 8 µg/mL inozivikanwa yeUSP Sodium Chloride RS, 4µg/mL ye4-hydroxybutane-1-sulfonic acid, uye 4 µg/mL yebis(4-sulfobutyl) ether disodium.
Sample solution: 4 mg/mL yeBetadex Sulfobutyl Ether Sodium
Chromatographic system
(Ona Chromatography <621>, System Suitability uye Ion Chromatography <1065>.)
Modhi: IC
Detector: Conductivity
Range: 30 µS
Iye zvino: 100 mA
Column: [Cherechedza-Pakupera kwekumhanya kwega kwega, chenesa mbiru uchishandisa Column wash solution A pamwero wekuyerera we1 mL/min kwemaminetsi makumi matatu neshanu wobva washandisa Column wash solution B panguva imwechete yekuyerera kwe35 min.]
Guard: 4.0-mm × 5.0-cm anion-exchange;kurongedza L61
Analytical: 4.0-mm × 25-cm anion-exchange;kurongedza L61
Column tembiricha: 30 °
Mudzvanyiriri: Micromembrane anion autosuppressor1 kana yakakodzera kemikari kudzvinyirira system
Kudzvanyirira: Autosuppression
Kuyerera kweyero: 1.0 mL/min
Jekiseni saizi: 20 µL
Kukodzera kwehurongwa
Muenzaniso: Standard solution
[Cherechedza-Nguva dzekuchengeta dzinopihwa ruzivo chete.Nguva dzekuchengeta 4-hydroxybutane-1-sulfonate ion, chloride ion, uye bis(sulfobutyl) ether ion i1.0, 1.4, uye 8.6, zvichiteerana.]
Kukodzera zvinodiwa
Kugadzirisa: NLT 2.0
Kutsauswa kwechiyereko: NMT 10.0%
Analysis
Samples: Yakajairwa mhinduro uye Sample mhinduro
Verenga chikamu chesodium chloride, 4-hydroxybutane-1-sulfonic acid, kana bis(sulfobutyl) ether disodium muchikamu cheBetadex Sulfobutyl Ether Sodium yakatorwa:
Mhedzisiro = (rU/rS) × (CS/CU) × F × 100
rU = peak mhinduro ye sodium chloride, 4-hydroxybutane-1-sulfonic acid, kana bis(sulfobutyl) ether disodium kubva kuSample solution
rS = peak mhinduro ye sodium chloride, 4-hydroxybutane-1-sulfonic acid, kana bis(sulfobutyl) ether disodium kubva kune Standard solution
CS = concentration ye sodium chloride, 4-hydroxybutane-1-sulfonic acid, kana bis(sulfobutyl) ether disodium muStandard solution (µg/mL)
CU = kusangana kweBetadex Sulfobutyl Ether Sodium muSample solution (mg/mL)
F = shanduko (10−3 0 100 0 mg/µg)
Maitiro ekugamuchira
Sodium chloride: NMT 0.2%
4-Hydroxybutane-1-sulfonic acid: NMT 0.09%
Bis(sulfobutyl) ether disodium: NMT 0.05%
ZVIYEDZO ZVAKANAKA
BACTERIAL ENDOTOXINS TEST <85>: Chiyero chebhakitiriya endotoxins ndechekuti zvinodiwa pasi peiyo yakakodzera dosage fomu monograph (s) umo Betadex Sulfobutyl Ether Sodium inoshandiswa inogona kusangana.Apo iyo chinyorwa chinotaura kuti Betadex Sulfobutyl Ether Sodium inofanira kuiswa pasi pekuenderera mberi kwekugadzirisa panguva yekugadzirira mafomu ejekiseni, chiyero chebhakitiriya endotoxins ndechokuti chinodiwa pasi peiyo yakakodzera dosage fomu monograph (s) umo Betadex Sulfobutyl Ether Sodium inoshandiswa. inogona kusangana.
• MICROBIAL ENUMERATION TESTS <61> uye ZVIYEDZO ZVAKATAURWA MICROORGANISMS <62>: Huwandu hwehuwandu hwe aerobic microbial hahupfuuri 100 cfu/g, uye huwandu hweforoma hwakasanganiswa uye mbiriso haipfuure makumi mashanu cfu/g.Inosangana nezvinodiwa zvekuyedzwa kwekusavapo kweEscherichia coli.
• KUjeka KWEKUGADZIRA
Sample solution: 30% (w/v) mhinduro
Ongororo: Ongorora mhinduro yeSample uchishandisa bhokisi rakareruka pakatarisana nechena uye nhema kumashure, uye nyora kuvepo kwechero haze, fluorescence, faibha, mapikisi, kana imwe nyaya yekunze.
Maitiro ekugamuchira: Mhinduro yakajeka, uye yakasununguka kubva kune zvimedu zvekunze.
• AVERAGE DEGREE OF SUBSTITUTION
Run electrolyte: 30 mM benzoic acid uye yakagadziridzwa kune pH inokodzera chiridzwa chinoshandiswa nekuwedzera 100 mM tris(hydroxymethyl) aminomethane buffer.
[Cherechedza-Nekuda kwekusiyana pakati pemacapillaries, imwe chete inoshandiswa pasi rose electrolyte pH haina kutaurwa.
Pane kudaro, iyo yakakwana pH yakabatana neyega yega capillary inofanirwa kutariswa zvinoenderana neiyo chiridzwa bhuku.]
Mushonga wakakwana: 10 mg/mL yeUSP Betadex Sulfobutyl Ether Sodium RS
Sample solution: 10 mg/mL yeBetadex Sulfobutyl Ether Sodium
Capillary rinsing maitiro: Shandisa akasiyana run electrolyte vials ye capillary rinse uye sampuli yekuongorora.Ita pre-analysis rinses zuva nezuva pamberi pekuongorora kwega kwega: simbura capillary ne 0.1 N sodium hydroxide kwemaminitsi makumi matatu, nemvura yeNLT 2 h, uye neRun electrolyte yeNLT 1 h.Ita pre-injection rinses pamberi pejekiseni rega rega sezvinotevera.Sukurudza capillary ne 0.1 N sodium hydroxide yeNLT 1 min, uye ne Run electrolyte yeNLT 3 min.Kana iyo capillary itsva iri kushandiswa, kuwedzera kune rinses nguva dzose inotsanangurwa pamusoro apa, itsva capillary inoda kuchenesa isati yatanga kushandiswa.Sukurudza capillary itsva ne 1 M sodium hydroxide kwe 1 h, ichiteverwa ne 2-h yekugeza mvura.
Electrophoretic system
(Ona Capillary Electrophoresis <1053>.)
Mode: High-performance CE
Detector: Inverse UV 200 nm, ine bandwidth ye20nm.[Cherechedza-Kuona wavelength ye205 nm ine bandwidth ye10 nm inogona kushandiswa seimwe nzira.]
Column: Sodium Peaks I–X (% Peak Area) 50-µm × 50-cm yakasanganiswa silica column
Column tembiricha: 25 °
Inoshandiswa voltage: 0.00 kusvika +30.00 kV linear ramp pamusoro pegumi maminetsi, ipapo pa30 kV kwemamwe 20 min.
Jekiseni saizi: Mavhoriyamu akaenzana pa 0.5 psi yegumi s
Kukodzera kwehurongwa
Muenzaniso: Standard solution
[Cherechedza-Ona Tafura 6 yenguva inofungidzirwa yekufamba kwebetadex sulfobutyl ether sodium peaks I-X (betadex sulfobutyl ether sodium peaks I, II, III, ..., X, ine beta cyclodextrin molecule ine 1, 2, 3, ..., 10 sulfobutyl substituent(s), zvichiteerana).Idzo nguva dzekutama ndedzezvinangwa zveruzivo chete kubatsira mukuzivikanwa kwepamusoro.]
Tafura 6

Kukodzera zvinodiwa
Chisarudzo: NLT 0.9, pakati pe betadex sulfobuty ether sodium peak IX uye betadex sulfobutyl ether sodium peak X
Analysis
Samples: Run electrolyte, mvura, Standard solution, uye Sample solution
Bayira iyo Standard solution uye Sample solution nekushandisa differential pressure ye 0.5 psi, yakaenzana ne 34 mbar, for 10 s, ichiteverwa nejekiseni reRun electrolyte pa 0.5 psi kwe 2 s.[Cherechedza-Majekiseni ePressure anofanira kuitwa nebhodhoro remvura kana Run electrolyte panoperera capillary.]
Rekodha maelectropherograms, uye woyera mhinduro dzepamusoro dzebetadex sulfobutyl ether sodium peaks (I kusvika X).Verenga iyo yakagadziriswa peak nzvimbo, AI, kune yega yega yepamusoro mueletropherogram:
Yakagadziriswa Peak Area A = Peak Area x Inoshanda Capillary Length (cm) / Nguva Yekufamba
Gadzirisa nzvimbo dzepamusoro dzakagadziriswa nekupa imwe neimwe sechikamu cheiyo yakazara yakagadziriswa nzvimbo yehamvuropu:
Nomalised Area, NA: A / n∑i=1 Ai x 100
n = mwero wepamusoro wekutsiva
Sarudza avhareji yedhigirii yekutsiva:
Avhareji yeDhigirii reKutsiva = n∑i = 1 (Chiyero cheKutsiva Peak x NA) / 100
Maitiro ekugamuchira: 6.2 ~ 6.9 yeavhareji degree yekutsiva
Kune imwe neimwe yebetadex sulfobutyl ether sodium peaks I-X, ona muganhu wepakati (% peak area) muTebhu 7.
Tafura 7

• PH <791>: 4.0-6.8, mune 30% (w/v) mhinduro mumvura isina carbon dioxide
• KUTARISA MVURA, Nzira I <921>: NMT 10.0%
ZVIMWE ZVINODIWA
• KUPAKIRA UYE KUCHENGESHA: Chengetedza mumidziyo yakavharwa zvakanaka, uye chengeta patembiricha yemumba.Dzivirira kubva pakunyorova.
• KUITA ILEBORO: Inyore kuratidza kushandiswa kwayo mukugadzira mafomu ekubaya jekiseni.
• USP REFERENCE ZVINHU <11>
USP Beta Cyclodextrin RS
USP Betadex Sulfobutyl Eteri Sodium RS
USP Endotoxin RS
USP Sodium Chloride RS■1S (NF30)