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 when n = 6.5
Beta cyclodextrin sulfobutyl ethers, sodium ntsev;
Beta cyclodextrin sulfobutyl ether sodium [182410-00-0].
DEFINITION
Betadex Sulfobutyl Ether Sodium yog npaj los ntawm alkylation ntawm betadex siv 1,4-butane sultone nyob rau hauv tej yam kev mob.
Qhov nruab nrab ntawm kev hloov pauv hauv betadex yog NLT 6.2 thiab NMT 6.9.
Nws muaj NLT 95.0% thiab NMT 105.0% ntawm C42H70−nO35 · (C4H8SO3Na)n (n = 6.2–6.9), xam ntawm lub hauv paus anhydrous.
IDENTIFICATION
• A. INFRARED ABSORPTION <197K>
• B. Lub sij hawm tuav ntawm lub ncov loj ntawm cov qauv kev daws teeb meem sib raug rau cov txheej txheem kev daws teeb meem, raws li tau txais hauv Assay.
• C. Nws ua tau raws li qhov yuav tsum tau ua ntawm kev xeem rau Qhov Nruab Nrab Degree ntawm Kev Hloov Kho.
• D. KEV KAWM TXUJ CI-GENERAL, Sodium 〈191〉
QHIA
• KEV PAB CUAM
Txawb theem: 0.1 M potassium nitrate hauv kev sib xyaw ntawm acetonitrile thiab dej (1: 4)
Kev daws teeb meem: 10 mg / mL ntawm USP Betadex Sulfobutyl Ether Sodium RS nyob rau theem txawb
Cov qauv tshuaj: 10 mg / mL ntawm Betadex Sulfobutyl Ether Sodium hauv Mobile Phase
Chromatographic system
(Saib Chromatography <621>, System Suitability.)
Qauv: LC
Detector: Refractive Index
Kev ntsuas kub: 35 ± 2 °
Kem: 7.8-mm × 30-cm analytical kem;kev l37.[CEEB TOOM-Yau cov kem nrog kev daws ntawm acetonitrile thiab dej (1: 9) thaum ua tiav ntawm kev khiav haujlwm.]
Tus nqi ntws: 1.0 mL / min
Kev txhaj tshuaj loj: 20 µL
Qhov system haum.
Qauv: Standard tov
Suitability xav tau
Tus txheeb ze tus qauv sib txawv: NMT 2.0%
Kev tsom xam
Qauv: Cov qauv kev daws teeb meem thiab cov qauv kev daws teeb meem
Xam cov feem pua ​​​​ntawm Betadex Sulfobutyl Ether Sodium [C42H70-nO35 · (C4H8SO3Na)n] hauv feem ntawm Betadex Sulfobutyl Ether Sodium noj:
Result = (rU/rS) × (CS/CU) × 100
rU = ncov teb rau betadex sulfobutyl ether
sodium los ntawm cov qauv tshuaj
rS = ncov teb rau betadex sulfobutyl ether
sodium los ntawm Standard tov
CS = concentration ntawm USP Betadex Sulfobutyl Ether
Sodium RS nyob rau hauv Standard tov (mg / mL)
CU = concentration ntawm Betadex Sulfobutyl Ether Sodium nyob rau hauv cov qauv tov (mg / mL)
Kev lees txais cov qauv: 95.0% ~ 105.0% ntawm lub hauv paus anhydrous
IMPURITIES
• HEAVY METALS, Method II <231>: NMT 5 ppm
• LIMIT ntawm BETA CYCLODEXTRIN (BETADEX)
Kev daws A: 25 mM sodium hydroxide
Tshuaj B: 250 mM sodium hydroxide thiab 1 M potassium nitrate
Mobile theem: Saib Table 1.
Table 1

Kev daws teeb meem: 2 µg / mL ntawm USP Beta Cyclodextrin RS
Cov qauv tshuaj: 2 mg / mL ntawm Betadex Sulfobutyl Ether Sodium
Chromatographic system
(Saib Chromatography <621>, System Suitability thiab Ion Chromatography <1065>.)
Qauv: IC
Ntes: Pulsed amperometry (amperometric cell nrog kub ua hauj lwm electrode thiab nyiaj siv electrode)
Kem
Guard: 4.0-mm × 5-cm anion-pauv;kev l61
Kev tsom xam: 4.0-mm × 25-cm anion-exchange;
kev l61
Kem kub: 50 ± 2 °
Tus nqi ntws: 1.0 mL / min
Kev txhaj tshuaj loj: 20 µL
Waveform rau pulsed amperometric detector: Saib Table 2.
Rooj 2

Qhov system haum
Qauv: Standard tov
Suitability xav tau
Tus txheeb ze tus qauv sib txawv: NMT 5.0%
Kev tsom xam
Qauv: Cov qauv kev daws teeb meem thiab cov qauv kev daws teeb meem
Xam cov feem pua ​​​​ntawm beta cyclodextrin (betadex) hauv feem ntawm Betadex Sulfobutyl Ether Sodium noj:
Result = (rU/rS) × (CS/CU) × F × 100
rU = ncov teb rau beta cyclodextrin los ntawm cov qauv tov
rS = ncov teb rau beta cyclodextrin los ntawm Standard tov
CS = concentration ntawm USP Beta Cyclodextrin RS nyob rau hauv Standard tov (µg/mL)
CU = concentration ntawm Betadex Sulfobutyl Ether Sodium nyob rau hauv cov qauv tov (mg / mL)
F = conversion factor (10-3 mg/µg)
Kev lees txais: NMT 0.1%
• LIMIT 1,4-BUTANE SULTONE
Cov txheej txheem sab hauv: 0.25 µg / mL ntawm diethyl sulfone
Standard Tshuag tov A: 0.5 µg / mL ntawm 1,4-butane sultone
Standard Tshuag tov B: 1.0 µg / mL ntawm 1,4-butane sultone
Standard Tshuag tov C: 2.0 µg / mL ntawm 1,4-butane sultone
Cov qauv kev daws teeb meem: 250 mg / mL ntawm Betadex Sulfobutyl Ether Sodium hauv cov txheej txheem sab hauv
Cov tshuaj dawb, thiab cov qauv kev daws teeb meem A, B, C, thiab D:
Ua raws li Table 3 kom tso cov khoom ntim ntawm cov txheej txheem sab hauv, txhua qhov kev daws teeb meem Standard, Cov qauv hauv Tshuag, dej, los yog methylene chloride hauv txhua lub khob ntsuas raj nrog lub stopper.[CEEB TOOM-Ib tug ntsia hlau-capped, 10-mL xeem raj yog tsim nyog.] Sib tov rau ntawm ib tug vortex tov khoom txhua lub raj rau 30 s, thiab cia nws sawv ntsug li 5 feeb los yog kom txog thaum tiav kev sib cais ntawm theem.Extract cov organic theem rau hauv GC vial thiab foob.[CEEB TOOM-Nrog kev saib xyuas zoo siv qhov tsawg kawg nkaus ntawm aqueous theem.] Ntxiv qhov ntau ntawm 1,4-butane sultone hauv cov qauv kev daws teeb meem A, B, C, thiab D yog 0.5, 1.0, 2.0, thiab 0 µg, feem.
Table 3

[CEEB TOOM- Npaj tam sim ua ntej siv.]
Chromatographic system
(Saib Chromatography <621>, System Suitability.)
Qauv: GC
Detector: Nplaim ionization
Kem: 0.32-mm × 25-m fused-silica capillary kem;0.5-µm txheej ntawm theem G46
Kub
Ntes: 270 °
Qhov chaw txhaj tshuaj: 200 °
Kem: Saib qhov program kub hauv Table 4
Table 4
Qhov ntsuas kub pib (°) Qhov kub thiab txias (° / min) Qhov ntsuas kub kawg (°) Tuav lub sij hawm ntawm qhov ntsuas kub kawg (min)
100 10 200 -
200 35 270 5
Carrier gas: Helium, feem ntau ntawm 12 psi inlet siab
Kev txhaj tshuaj loj: 1.0 µL
Kev txhaj tshuaj: Splitless txhaj rau 0.5 min, ces faib ntawm 50 mL / min.[CEEB TOOM-Kev siv cov txheej txheem sib cais tsis tsim nyog tau pom zoo.]
Qhov system haum
Qauv: Sample tov B
[CEEB TOOM-Lub sij hawm tuav cov txheeb ze rau diethyl sulfone thiab 1,4-butane sultone yog 0.7 thiab 1.0, ntsig txog.]
Suitability xav tau
Tus txheeb ze tus qauv sib txawv: NMT 10.0%
Kev tsom xam
Cov Qauv: Cov tshuaj dawb, Cov qauv kev daws teeb meem A, B, C, thiab D
Kho qhov sib piv ntawm cov lus teb ncov ntawm 1,4-butane sultone rau diethyl sulfone hauv cov qauv tshuaj A, B, C, lossis D los ntawm kev rho tawm qhov piv ntawm cov lus teb ncov ntawm 1,4-butane sultone rau ethyl sulfone hauv cov tshuaj dawb. .Npaj qhov kho qhov sib piv ntawm cov lus teb ncov ntawm 1,4-butane sultone rau cov lus teb siab tshaj ntawm diethyl sulfone hauv cov tshuaj A, B, C lossis D, piv rau qhov ntau ntxiv, hauv µg, ntawm 1,4-butane sultone.Extrapolate kab koom nrog cov ntsiab lus ntawm daim duab kom txog rau thaum nws ua tau raws li qhov ntau axis.Qhov kev ncua deb ntawm qhov taw tes no thiab qhov kev sib tshuam ntawm cov axes sawv cev rau qhov ntau ntawm 1,4-butane sultone, A, hauv µg, hauv 4-mL feem ntawm Cov Qauv Tshuag Tshuaj.Xam cov ntsiab lus ntawm 1,4-butane sultone nyob rau hauv ib feem ntawm Betadex Sulfobutyl Ether Sodium noj:
Result = A/(VExt × CU × F)
A = txiav txim siab saum toj no
VExt = ntim ntawm cov qauv Tshuag tov siv nyob rau hauv lub extraction kauj ruam, 4.0 mL
CU = concentration ntawm Betadex Sulfobutyl Ether Sodium nyob rau hauv cov qauv Tshuag tov (mg / mL)
F = conversion factor (10-3 g/mg)
Kev lees txais: hydroxybutane-1-sulfonic acid, los yog NMT 0.5 ppm
• LIMIT SODIUM CHLORIDE, 4-HYDROXYBUTANE-1-SULFONIC ACID, thiab BIS (4-SULFOBUTYL) ETHER DISODIUM
Kev daws A: 5 mM sodium hydroxide, degas hauv lub nkoj kaw rau 15 min
Kev daws B: 25 mM sodium hydroxide, degas hauv lub nkoj kaw rau 15 min
Mobile theem: Saib Table 5
Table 5

Kem ntxuav kua A: 50 mM sodium citrate
Kem ntxuav kua B: 150 mM sodium hydroxide
Cov txheej txheem kev daws teeb meem: Npaj ib qho kev daws teeb meem uas paub tias muaj ntau ntawm 8 µg / mL ntawm USP Sodium Chloride RS, 4µg / mL ntawm 4-hydroxybutane-1-sulfonic acid, thiab 4 µg / mL ntawm bis (4-sulfobutyl) ether disodium.
Cov qauv tshuaj: 4 mg / mL ntawm Betadex Sulfobutyl Ether Sodium
Chromatographic system
(Saib Chromatography <621>, System Suitability thiab Ion Chromatography <1065>.)
Qauv: IC
Detector: conductivity
Ntev: 30 µS
Tam sim no: 100 mA
Kem: [CEEB TOOM-Thaum kawg ntawm txhua qhov kev khiav, ntxuav cov kab uas siv Kab Ntxuav A ntawm tus nqi ntws ntawm 1 mL / min rau 35 min ces siv Kab Ntxuav B ntawm tib tus nqi rau 35 min.]
Guard: 4.0-mm × 5.0-cm anion-pauv;kev l61
Kev tsom xam: 4.0-mm × 25-cm anion-exchange;kev l61
Kem kub: 30 °
Suppressor: Micromembrane anion autosuppressor1 los yog cov tshuaj tua kab mob tsim nyog
Suppressant: Autosuppression
Tus nqi ntws: 1.0 mL / min
Kev txhaj tshuaj loj: 20 µL
Qhov system haum
Qauv: Standard tov
[CEEB TOOM-Lub sij hawm tuav cov txheeb ze yog muab rau cov ntaub ntawv nkaus xwb.Lub sij hawm tuav cov txheeb ze rau 4-hydroxybutane-1-sulfonate ion, chloride ion, thiab bis (sulfobutyl) ether ion yog 1.0, 1.4, thiab 8.6, raws li.]
Suitability xav tau
Kev daws teeb meem: NLT 2.0
Tus txheeb ze tus qauv sib txawv: NMT 10.0%
Kev tsom xam
Qauv: Cov qauv kev daws teeb meem thiab cov qauv kev daws teeb meem
Xam cov feem pua ​​​​ntawm sodium chloride, 4-hydroxybutane-1-sulfonic acid, los yog bis (sulfobutyl) ether disodium nyob rau hauv ib feem ntawm Betadex Sulfobutyl Ether Sodium noj:
Result = (rU/rS) × (CS/CU) × F × 100
rU = ncov teb rau sodium chloride, 4-hydroxybutane-1-sulfonic acid, los yog bis (sulfobutyl) ether disodium los ntawm cov qauv tov
rS = ncov teb rau sodium chloride, 4-hydroxybutane-1-sulfonic acid, los yog bis (sulfobutyl) ether disodium los ntawm Standard tov
CS = concentration ntawm sodium chloride, 4-hydroxybutane-1-sulfonic acid, los yog bis (sulfobutyl) ether disodium hauv Standard tov (µg/mL)
CU = concentration ntawm Betadex Sulfobutyl Ether Sodium nyob rau hauv cov qauv tov (mg / mL)
F = conversion factor (10-3 0 100 0 mg/µg)
Kev lees txais
Sodium chloride: NMT 0.2%
4-Hydroxybutane-1-sulfonic acid: NMT 0.09%
Bis (sulfobutyl) ether disodium: NMT 0.05%
TSEEM CEEB
BACTERIAL ENDOTOXINS TEST <85>: Cov theem ntawm cov kab mob endotoxins yog xws li qhov yuav tsum tau nyob rau hauv daim ntawv ntau npaum li cas monograph (s) uas Betadex Sulfobutyl Ether Sodium yog siv tau.Qhov twg daim ntawv lo hais tias Betadex Sulfobutyl Ether Sodium yuav tsum tau ua ntxiv thaum lub sij hawm npaj cov tshuaj txhaj tshuaj, theem ntawm cov kab mob endotoxins yog xws li qhov yuav tsum tau nyob rau hauv daim ntawv muaj feem ntau npaum li cas monograph (s) uas Betadex Sulfobutyl Ether Sodium yog siv. tuaj yeem ntsib.
• MICROBIAL ENUMERATION TESTS <61> thiab TESTS FOR SPECIFIED MICROORGANISMS <62>: Tag nrho cov aerobic microbial suav tsis pub tshaj 100 cfu/g, thiab tag nrho cov pwm ua ke thiab cov poov xab suav tsis pub tshaj 50 cfu/g.Nws ua tau raws li qhov yuav tsum tau ua ntawm kev sim rau qhov tsis muaj Escherichia coli.
• Kev daws teeb meem meej
Sample tov: 30% (w/v) tov
Kev Ntsuam Xyuas: Tshawb xyuas cov qauv kev daws teeb meem uas siv lub teeb lub teeb tawm tsam dawb thiab dub keeb kwm yav dhau, thiab sau tseg tias muaj qhov kub hnyiab, fluorescence, fibers, specks, lossis lwm yam txawv teb chaws.
Kev lees txais cov qauv: Cov kev daws teeb meem yog qhov tseeb, thiab qhov tseem ceeb tsis pub muaj cov khoom txawv teb chaws.
• AVERAGE DEGREE OF SUBSTITUTION
Khiav electrolyte: 30 mM benzoic acid thiab hloov mus rau pH uas haum rau cov cuab yeej siv los ntawm kev sib ntxiv ntawm 100 mM tris (hydroxymethyl) aminomethane buffer.
[CEEB TOOM-Vim qhov txawv ntawm capillaries, ib qho kev siv hluav taws xob thoob ntiaj teb pH tsis tau teev tseg.
Hloov chaw, qhov zoo tshaj pH cuam tshuam nrog txhua tus neeg capillary yuav tsum tau txiav txim siab raws li phau ntawv qhia.]
Kev daws teeb meem: 10 mg / mL ntawm USP Betadex Sulfobutyl Ether Sodium RS
Cov qauv tshuaj: 10 mg / mL ntawm Betadex Sulfobutyl Ether Sodium
Capillary rinsing txheej txheem: Siv cais khiav electrolyte vials rau capillary yaug thiab coj mus kuaj.Ua ntej kev soj ntsuam yaug txhua hnub ua ntej txhua qhov kev tshuaj ntsuam: yaug lub capillary nrog 0.1 N sodium hydroxide rau 30 min, nrog dej rau NLT 2 h, thiab khiav electrolyte rau NLT 1 h.Ua ntej txhaj tshuaj yaug ua ntej txhua qhov kev txhaj tshuaj raws li hauv qab no.Yaug lub capillary nrog 0.1 N sodium hydroxide rau NLT 1 min, thiab nrog Run electrolyte rau NLT 3 min.Yog tias siv cov capillary tshiab, ntxiv rau cov tshuaj yaug li niaj zaus tau piav qhia saum toj no, lub capillary tshiab yuav tsum tau yaug ua ntej nws siv thawj zaug.Yaug lub capillary tshiab nrog 1 M sodium hydroxide rau 1 h, ua raws li 2-h dej yaug.
Electrophoretic system
(Saib Capillary Electrophoresis <1053>.)
Hom: Kev ua haujlwm siab CE
Ntes: Inverse UV 200 nm, nrog bandwidth ntawm 20nm.[CEEB TOOM-Kev kuaj pom wavelength ntawm 205 nm nrog bandwidth ntawm 10 nm tuaj yeem siv los ua lwm txoj hauv kev.]
Kem: Sodium Peaks I–X (% Peak Area) 50-µm × 50-cm fused silica kem
Kem kub: 25 °
Kev siv hluav taws xob: 0.00 txog + 30.00 kV linear ramp tshaj 10 min, tom qab ntawd ntawm 30 kV rau 20 min ntxiv
Kev txhaj tshuaj loj: Sib npaug ntawm 0.5 psi rau 10 s
Qhov system haum
Qauv: Standard tov
[CEEB TOOM-Saib Daim duab 6 rau qhov kwv yees kwv yees lub sij hawm tsiv teb tsaws chaw rau betadex sulfobutyl ether sodium peaks I-X (betadex sulfobutyl ether sodium peaks I, II, III, ..., X, muaj beta cyclodextrin molecule nrog 1, 2, 3, ..., 10 sulfobutyl substituent(s), feem).Lub sij hawm tsiv teb tsaws chaw txheeb ze yog rau cov ntaub ntawv xov xwm nkaus xwb los pab hauv kev txheeb xyuas qhov siab tshaj.]
Table 6

Suitability xav tau
Kev daws teeb meem: NLT 0.9, nruab nrab ntawm Betadex sulfobuty ether sodium ncov IX thiab Betadex sulfobutyl ether sodium ncov X
Kev tsom xam
Qauv: Khiav electrolyte, dej, Standard tov, thiab Sample tov
Txhaj cov tshuaj Standard thiab cov qauv kev daws teeb meem los ntawm kev siv lub siab sib txawv ntawm 0.5 psi, sib npaug rau 34 mbar, rau 10 s, ua raws li kev txhaj tshuaj ntawm Khiav electrolyte ntawm 0.5 psi rau 2 s.[CEEB TOOM-Kev txhaj tshuaj yuav tsum tau ua nrog lub vial ntawm dej lossis Khiav electrolyte ntawm qhov hluav taws xob kawg ntawm capillary.]
Sau cov electropherograms, thiab ntsuas lub ncov cov lus teb rau tus neeg betadex sulfobutyl ether sodium peaks (I txog X).Xam qhov kho qhov chaw ncov, AI, rau txhua lub ncov hauv eletropherogram:
Kho Peak Area A = Peak Area x Zoo Capillary Length (cm) / Lub Sijhawm Migration
Normalize qhov kho qhov chaw siab tshaj plaws los ntawm kev nthuav qhia txhua qhov feem pua ​​​​ntawm tag nrho qhov chaw hloov kho lub hnab ntawv:
Nomalized Area, NA: A / n∑i = 1 Ai x 100
n = qib siab tshaj ntawm kev hloov pauv
Txiav txim siab qhov nruab nrab ntawm kev hloov pauv:
Nruab Nrab Degree of Hloov = n∑i = 1 (Qib Hloov rau Peak x NA) / 100
Kev lees txais: 6.2 ~ 6.9 rau qhov nruab nrab ntawm kev hloov pauv
Rau txhua qhov ntawm betadex sulfobutyl ether sodium peaks I-X, saib qhov txwv ntau (% ncov cheeb tsam) hauv Table 7.
Table 7

• PH <791>: 4.0-6.8, hauv 30% (w/v) tov hauv dej tsis muaj carbon dioxide
• KEV TIV THAIV DUA, Txoj Kev I <921>: NMT 10.0%
TSEEM CEEB
• PACKAGING THIAB STORAGE: Khaws rau hauv cov thawv kaw kom zoo, thiab khaws cia hauv chav sov.Tiv thaiv los ntawm noo noo.
• LABELING: Sau npe los qhia nws siv hauv kev tsim cov ntawv txhaj tshuaj.
• USP REFERENCE STANDARDS <11>
USP Beta Cyclodextrin RS
USP Betadex Sulfobutyl Ether Sodium RS
Tom ntej: USP Endotoxin RS
USP Sodium Chloride RS■1S (NF30)