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

Betadex Sulfobutyl Eteri iṣuu soda
C42H70-nO35 · (C4H8SO3Na) n 2163 nigbati n = 6.5
Beta cyclodextrin sulfobutyl ethers, iṣuu soda;
Beta cyclodextrin sulfobutyl ether sodium [182410-00-0].
ITUMO
Betadex Sulfobutyl Ether Sodium ti pese sile nipasẹ alkylation ti betadex lilo 1,4-butane sultone labẹ awọn ipo ipilẹ.
Iwọn aropin ti aropo ni betadex jẹ NLT 6.2 ati NMT 6.9.
O ni NLT 95.0% ati NMT 105.0% ti C42H70-nO35 · (C4H8SO3Na) n (n = 6.2–6.9), iṣiro lori ipilẹ anhydrous.
Ìdámọ̀
• A. INFRED ABSORPTION <197K>
• B. Awọn akoko idaduro ti awọn pataki tente oke ti awọn Ayẹwo ojutu ni ibamu si ti awọn boṣewa ojutu, bi gba ninu awọn Assay.
• C. O pade awọn ibeere ti idanwo naa fun Iwọn Apapọ Iyipada.
D. Awọn idanwo idanimọ-Gbogbogbo, Sodium 〈191〉
ASAY
• Ilana
Ipele alagbeka: iyọ potasiomu 0.1 M ninu adalu acetonitrile ati omi (1: 4)
Ojutu boṣewa: 10 mg/mL ti USP Betadex Sulfobutyl Ether Sodium RS ni apakan Alagbeka
Ojutu ayẹwo: 10 mg/mL ti Betadex Sulfobutyl Ether Sodium ni alakoso Alagbeka
Eto Chromatographic
(Wo Chromatography <621>, Ibamu Eto.)
Ipo: LC
Oluwadi: Refractive Ìwé
Iwọn otutu oluwari: 35 ± 2°
Ọwọn: 7.8-mm × 30-cm ọwọn atupale;iṣakojọpọ L37.[AKIYESI-Fi omi ṣan ọwọn pẹlu ojutu ti acetonitrile ati omi (1: 9) ni ipari ti jara ṣiṣe.]
Oṣuwọn sisan: 1.0 milimita / min
Iwọn abẹrẹ: 20µL
Ibamu eto.
Apeere: Standard ojutu
Awọn ibeere ibamu
Iyatọ boṣewa ibatan: NMT 2.0%
Onínọmbà
Awọn apẹẹrẹ: Ojutu boṣewa ati ojutu Ayẹwo
Ṣe iṣiro ipin ti betadex sulfobutyl ether sodium [C42H70-nO35 · (C4H8SO3Na) n] ni apakan ti Betadex Sulfobutyl Ether Sodium ti o mu:
Esi = (rU/rS) × (CS/CU) × 100
rU = esi to ga julọ fun betadex sulfobutyl ether
iṣuu soda lati ojutu Ayẹwo
rS = idahun ti o ga julọ fun betadex sulfobutyl ether
iṣuu soda lati ojutu Standard
CS = ifọkansi ti USP Betadex Sulfobutyl Ether
Iṣuu soda RS ni ojutu Standard (mg/ml)
CU = ifọkansi ti Betadex Sulfobutyl Ether Sodium ninu ojutu Ayẹwo (mg/mL)
Awọn ibeere gbigba: 95.0% ~ 105.0% lori ipilẹ anhydrous
ALÁÌṢẸ́
• Awọn irin eru, Ọna II <231>: NMT 5 ppm
OPIN TI BETA CYCLODEXTRIN (BETADEX)
Solusan A: 25 mM sodium hydroxide
Solusan B: 250 mM sodium hydroxide ati 1 M potasiomu iyọ
Ipele Alagbeka: Wo Tabili 1.
Tabili 1

Ojutu boṣewa: 2 µg/ml ti USP Beta Cyclodextrin RS
Ojutu ayẹwo: 2 mg/mL ti Betadex Sulfobutyl Ether Sodium
Eto Chromatographic
(Wo Chromatography <621>, Imudara eto ati Ion Chromatography <1065>.)
Ipo: IC
Oluwari: amperometry pulsed (ẹyin amperometric pẹlu elekiturodu ti n ṣiṣẹ goolu ati elekiturodu itọkasi fadaka)
Àwọ̀n
Oluso: 4.0-mm × 5-cm anion-paṣipaarọ;iṣakojọpọ L61
Itupalẹ: 4.0-mm × 25-cm anion-paṣipaarọ;
iṣakojọpọ L61
Iwọn otutu: 50 ± 2°
Oṣuwọn sisan: 1.0 milimita / min
Iwọn abẹrẹ: 20µL
Waveform fun aṣawari amperometric pulsed: Wo Tabili 2.
Tabili 2

Ibamu eto
Apeere: Standard ojutu
Awọn ibeere ibamu
Iyatọ boṣewa ibatan: NMT 5.0%
Onínọmbà
Awọn apẹẹrẹ: Ojutu boṣewa ati ojutu Ayẹwo
Ṣe iṣiro ipin ti beta cyclodextrin (betadex) ni apakan ti Betadex Sulfobutyl Ether Sodium ti o mu:
Esi = (rU/rS) × (CS/CU) × F × 100
rU = idahun ti o ga julọ fun beta cyclodextrin lati inu ojutu Ayẹwo
rS = idahun ti o ga julọ fun beta cyclodextrin lati ojutu Standard
CS = ifọkansi ti USP Beta Cyclodextrin RS ni ojutu Standard (µg/ml)
CU = ifọkansi ti Betadex Sulfobutyl Ether Sodium ninu ojutu Ayẹwo (mg/mL)
F = ifosiwewe iyipada (10-3 mg/µg)
Ilana gbigba: NMT 0.1%
• OPIN OF 1,4-BUTANE SULTONE
Ti abẹnu boṣewa ojutu: 0,25 µg/ml ti diethyl sulfone
Ojutu ọja iṣura boṣewa A: 0.5 µg/mL ti sultone 1,4-butane
Ojutu ọja iṣura boṣewa B: 1.0 µg/ml ti sultone 1,4-butane
Ojutu ọja iṣura boṣewa C: 2.0 µg/ml ti sultone 1,4-butane
Ojutu ọja ayẹwo: 250 mg/mL ti Betadex Sulfobutyl Ether Sodium ninu ojutu boṣewa inu inu
Ojutu òfo, ati Awọn ojutu Ayẹwo A, B, C, ati D:
Tẹle Tabili 3 lati gbe awọn iwọn ti ojutu boṣewa inu, ojutu Ọja Ọja kọọkan, Ayẹwo iṣura ojutu, omi, tabi methylene kiloraidi ninu tube idanwo gilasi kọọkan pẹlu iduro kan.[AKIYESI-A skru-capped, 10-mL test tube ni o dara.] Illa lori aladapọ vortex kan tube idanwo kọọkan fun 30 s, ki o jẹ ki o duro fun o kere ju 5 min tabi titi ti o fi jẹ iyatọ ti ipele naa.Jade ipele Organic sinu vial GC kan ati edidi.[AKIYESI-Pẹlu iṣọra nla gba iye ti o kere julọ ti ipele olomi.] Awọn iwọn ti a ṣafikun ti sultone 1,4-butane ni Awọn solusan Ayẹwo A, B, C, ati D jẹ 0.5, 1.0, 2.0, ati 0 µg, lẹsẹsẹ.
Tabili 3

[AKIYESI-Mura lẹsẹkẹsẹ ṣaaju lilo.]
Eto Chromatographic
(Wo Chromatography <621>, Ibamu Eto.)
Ipo: GC
Oluwadi: ina ionization
Ọwọn: 0.32-mm × 25-m fused-silica capillary column;0.5-µm Layer ti alakoso G46
Iwọn otutu
Awari: 270°
Ibudo abẹrẹ: 200°
Ọwọn: Wo eto iwọn otutu ni Tabili 4
Tabili 4
Iwọn otutu akọkọ (°) Ramp Iwọn otutu (°/min) Iwọn otutu ikẹhin (°) Aago Daduro ni Ipari otutu (min)
100 10 200 -
200 35 270 5
Gaasi ti ngbe: Helium, ni igbagbogbo ni titẹ 12 psi titẹsi
Iwọn abẹrẹ: 1.0 µL
Iru abẹrẹ: Abẹrẹ ti ko ni pipin fun iṣẹju 0.5, lẹhinna pin ni 50 mL/min.[AKIYESI-Lilo laini abẹrẹ ti ko ni pipin ti o yẹ ni a gbaniyanju.]
Ibamu eto
Apeere: Apeere ojutu B
[AKIYESI-Awọn akoko idaduro ibatan fun diethyl sulfone ati 1,4-butane sultone jẹ 0.7 ati 1.0, lẹsẹsẹ.]
Awọn ibeere ibamu
Iyatọ boṣewa ibatan: NMT 10.0%
Onínọmbà
Awọn apẹẹrẹ: Ojutu òfo, Awọn ojutu Ayẹwo A, B, C, ati D
Ṣe atunṣe ipin ti awọn idahun tente oke ti sultone 1,4-butane si diethyl sulfone ni Ayẹwo Ayẹwo A, B, C, tabi D nipa iyokuro ipin ti awọn idahun ti o ga julọ ti sultone 1,4-butane si ethyl sulfone ninu ojutu òfo .Pirodi ipin ti a ṣe atunṣe ti idahun tente oke ti 1,4-butane sultone si idahun tente oke ti diethyl sulfone ni Ayẹwo Ayẹwo A, B, C tabi D, ni ibamu si iye ti a ṣafikun, ni µg, ti 1,4-butane sultone.Extrapolate ila ti o darapọ mọ awọn aaye lori iyaya titi yoo fi pade ipo iwọn.Aaye laarin aaye yii ati ikorita ti awọn aake duro fun opoiye sultone 1,4-butane, A, ni µg, ni apakan 4-mL ti ojutu ọja iṣura.Ṣe iṣiro akoonu ti sultone 1,4-butane ni apakan ti Betadex Sulfobutyl Ether Sodium ti o mu:
Esi = A/(VExt × CU × F)
A = pinnu loke
VExt = iwọn didun ti ojutu ọja iṣura Ayẹwo ti a lo ninu igbesẹ isediwon, 4.0 milimita
CU = ifọkansi ti Betadex Sulfobutyl Ether Sodium ninu ojutu iṣura Ayẹwo (mg/mL)
F = ifosiwewe iyipada (10-3 g/mg)
Awọn ilana gbigba: hydroxybutane-1-sulfonic acid, tabi NMT 0.5 ppm
• OPIN SODIUM chloride, 4-HYDROXYBUTANE-1-SULFONIC ACID, ATI BIS (4-SULFOBUTYL) ETHER DISODIUM.
Solusan A: 5 mM sodium hydroxide, degas ni ohun elo ti a ti pa fun 15 min
Solusan B: 25 mM sodium hydroxide, degas ni ohun elo ti a ti pa fun 15 min
Ipele Alagbeka: Wo Tabili 5
Tabili 5

Ojutu fifọ ọwọn A: 50 mM sodium citrate
Ojutu fifọ ọwọn B: 150 mM sodium hydroxide
Ojutu boṣewa: Mura ojutu kan nini awọn ifọkansi ti a mọ ti 8 µg/mL ti USP Sodium Chloride RS, 4µg/mL ti 4-hydroxybutane-1-sulfonic acid, ati 4 µg/mL ti bis (4-sulfobutyl) ether disodium.
Ojutu ayẹwo: 4 mg/mL ti Betadex Sulfobutyl Ether Sodium
Eto Chromatographic
(Wo Chromatography <621>, Imudara eto ati Ion Chromatography <1065>.)
Ipo: IC
Oluwadi: Iwa
Iwọn: 30µS
Lọwọlọwọ: 100 mA
Ọwọn: [AKIYESI-Ni ipari ṣiṣe kọọkan, nu ọwọn naa nipa lilo ojutu fifọ iwe A ni iwọn sisan ti 1 milimita / min fun awọn iṣẹju 35 lẹhinna lilo ojutu fifọ iwe B ni iwọn sisan kanna fun awọn iṣẹju 35.]
Oluso: 4.0-mm × 5.0-cm anion-paṣipaarọ;iṣakojọpọ L61
Itupalẹ: 4.0-mm × 25-cm anion-paṣipaarọ;iṣakojọpọ L61
Iwọn otutu: 30°
Suppressor: Micromembrane anion autosuppressor1 tabi eto imukuro kemikali to dara
Suppressant: Autosuppression
Oṣuwọn sisan: 1.0 milimita / min
Iwọn abẹrẹ: 20µL
Ibamu eto
Apeere: Standard ojutu
[AKIYESI-Awọn akoko idaduro ibatan ni a pese fun alaye nikan.Awọn akoko idaduro ojulumo fun 4-hydroxybutane-1-sulfonate ion, chloride ion, ati bis(sulfobutyl) ether ion jẹ 1.0, 1.4, ati 8.6, lẹsẹsẹ.]
Awọn ibeere ibamu
Ipinnu: NLT 2.0
Iyatọ boṣewa ibatan: NMT 10.0%
Onínọmbà
Awọn apẹẹrẹ: Ojutu boṣewa ati ojutu Ayẹwo
Ṣe iṣiro ipin ogorun iṣuu soda kiloraidi, 4-hydroxybutane-1-sulfonic acid, tabi bis(sulfobutyl) ether disodium ni ipin ti Betadex Sulfobutyl Ether Sodium ti o mu:
Esi = (rU/rS) × (CS/CU) × F × 100
rU = esi ti o ga julọ fun iṣuu soda kiloraidi, 4-hydroxybutane-1-sulfonic acid, tabi bis (sulfobutyl) ether disodium lati inu ojutu Ayẹwo
rS = idahun ti o ga julọ fun iṣuu soda kiloraidi, 4-hydroxybutane-1-sulfonic acid, tabi bis (sulfobutyl) ether disodium lati ojutu Standard
CS = ifọkansi ti iṣuu soda kiloraidi, 4-hydroxybutane-1-sulfonic acid, tabi bis (sulfobutyl) ether disodium ninu ojutu Standard (µg/ml)
CU = ifọkansi ti Betadex Sulfobutyl Ether Sodium ninu ojutu Ayẹwo (mg/mL)
F = ifosiwewe iyipada (10-3 0 100 miligiramu/µg)
Awọn ilana gbigba
Sodium kiloraidi: NMT 0.2%
4-Hydroxybutane-1-sulfonic acid: NMT 0.09%
Bis(sulfobutyl) ether disodium: NMT 0.05%
Awọn idanwo pataki
Idanwo BACTERIAL ENDOTOXINS <85>: Ipele ti awọn endotoxins kokoro arun jẹ iru pe ibeere labẹ iwọn lilo fọọmu monograph (s) ti o yẹ ninu eyiti Betadex Sulfobutyl Ether Sodium ti lo le pade.Nibo aami naa ti sọ pe Betadex Sulfobutyl Ether Sodium gbọdọ wa ni labẹ sisẹ siwaju lakoko igbaradi ti awọn fọọmu iwọn lilo injectable, ipele ti endotoxins kokoro jẹ iru pe ibeere labẹ iwọn lilo iwọn lilo monograph (s) ti o yẹ ninu eyiti Betadex Sulfobutyl Ether Sodium ti lo. le pade.
• Awọn idanwo Iṣiro MICROBIAL <61> ati awọn idanwo FUN PATAKI MICROORGANISMS <62>: Lapapọ kika aerobic microbial ko kọja 100 cfu/g, ati pe apapọ awọn molds ati iwukara apapọ ko kọja 50 cfu/g.O pade awọn ibeere ti idanwo fun isansa ti Escherichia coli.
• ITOJU OJUTU
Apeere ojutu: 30% (w / v) ojutu
Onínọmbà: Ṣe ayẹwo ojutu Ayẹwo nipa lilo apoti ina kan lodi si awọn ipilẹ funfun ati dudu, ki o ṣe igbasilẹ wiwa eyikeyi haze, fluorescence, awọn okun, awọn ẹiyẹ, tabi ọrọ ajeji miiran.
Awọn ibeere gbigba: Ojutu naa han gbangba, ati ni pataki ni ominira lati awọn patikulu ti ọrọ ajeji.
• Apapọ ìyí ti aropo
Ṣiṣe electrolyte: 30 mM benzoic acid ati ṣatunṣe si pH ti o dara fun ohun elo ti a lo nipasẹ afikun 100 mM tris (hydroxymethyl) aminomethane buffer.
[AKIYESI-Nitori iyatọ laarin awọn capillaries, pH electrolyte kan ti o wulo fun gbogbo agbaye ko ni pato.
Dipo, pH ti o dara julọ ti o ni nkan ṣe pẹlu olukaluku kọọkan yẹ ki o pinnu ni ibamu si itọnisọna ohun elo.]
Ojutu boṣewa: 10 mg/mL ti USP Betadex Sulfobutyl Ether Sodium RS
Ojutu ayẹwo: 10 mg / mL ti Betadex Sulfobutyl Ether Sodium
Ilana fifin capillary: Lo awọn lẹgbẹrun elekitiroti ṣiṣe lọtọ fun omi ṣan capillary ati itupalẹ ayẹwo.Ṣe awọn ṣan omi-iṣaaju iṣaju ni ipilẹ ojoojumọ ṣaaju itupalẹ kọọkan: fi omi ṣan capillary pẹlu 0.1 N sodium hydroxide fun 30 min, pẹlu omi fun NLT 2 h, ati pẹlu Run electrolyte fun NLT 1 h.Ṣe awọn ṣan omi abẹrẹ ṣaaju si abẹrẹ kọọkan gẹgẹbi atẹle.Fi omi ṣan awọn capillary pẹlu 0.1 N sodium hydroxide fun NLT 1 min, ati pẹlu Run electrolyte fun NLT 3 min.Ti o ba ti lo capillary tuntun, ni afikun si awọn ṣan omi deede ti a ṣalaye loke, capillary tuntun nilo omi ṣan ṣaaju lilo akọkọ rẹ.Fi omi ṣan omi titun pẹlu 1 M sodium hydroxide fun 1 wakati, tẹle pẹlu omi ṣan omi 2-h.
Electrophoretic eto
(Wo Capillary Electrophoresis <1053>.)
Ipo: Iṣẹ-giga CE
Oluwari: Inverse UV 200 nm, pẹlu bandiwidi kan ti 20nm.[AKIYESI-Iwọn igbi wiwa ti 205 nm pẹlu bandiwidi ti 10 nm le ṣee lo bi yiyan.]
Àwọ̀n: Sodium Peaks I–X (% Agbegbe tente oke) 50-µm × 50-cm ọwọn siliki ti a dapọ
Iwọn otutu ti ọwọn: 25°
Foliteji ti a lo: 0.00 si + 30.00 kV rampu laini lori iṣẹju 10, lẹhinna ni 30 kV fun iṣẹju 20 siwaju sii
Iwọn abẹrẹ: Awọn iwọn dogba ni 0.5 psi fun awọn iṣẹju 10
Ibamu eto
Apeere: Standard ojutu
[AKIYESI-Wo Tabili 6 fun awọn akoko ijira ojulumo isunmọ fun betadex sulfobutyl ether sodium tente oke I–X (betadex sulfobutyl ether sodium peaks I, II, III, ..., X, ni moleku beta cyclodextrin pẹlu 1, 2, 3, ..., 10 sulfobutyl aropo(s), lẹsẹsẹ).Awọn akoko ijira ibatan jẹ fun awọn idi alaye nikan lati ṣe iranlọwọ ni idanimọ ti o ga julọ.]
Tabili 6

Awọn ibeere ibamu
Ipinnu: NLT 0.9, laarin betadex sulfobuty ether sodium peak IX ati betadex sulfobutyl ether sodium tente oke X
Onínọmbà
Awọn apẹẹrẹ: Ṣiṣe awọn elekitiroti, omi, ojutu boṣewa, ati ojutu Ayẹwo
Abẹrẹ ojutu Standard ati ojutu Ayẹwo nipa lilo titẹ iyatọ ti 0.5 psi, deede si 34 mbar, fun 10 s, atẹle nipa abẹrẹ ti Run electrolyte ni 0.5 psi fun 2 s.[AKIYESI-Tẹ awọn abẹrẹ yẹ ki o ṣe pẹlu vial ti omi tabi Ṣiṣe elekitiroti ni opin iṣan jade ti capillary.]
Gba awọn elekitirogira silẹ, ki o si wọn awọn idahun ti o ga julọ fun ẹnikọọkan betadex sulfobutyl ether sodium tente oke (I si X).Ṣe iṣiro agbegbe tente oke ti a ṣe atunṣe, AI, fun oke kọọkan ninu eletropherogram:
Agbegbe tente oke Atunse A = Agbegbe tente oke x Gigun Kapila ti o munadoko (cm) / Akoko Iṣiwa
Ṣe deede awọn agbegbe tente oke ti a ṣe atunṣe nipa fifihan ọkọọkan bi ipin ogorun ti agbegbe apoowe atunṣe lapapọ:
Agbegbe ti a fi orukọ silẹ, NA: A / n∑i=1 Ai x 100
n = ipele ti o ga julọ ti aropo
Ṣe ipinnu aropin iwọn aropo:
Apapọ Iwọn Iyipo = n∑i=1 (Ipele ti Fidipo fun Peak x NA) / 100
Awọn ibeere gbigba: 6.2 ~ 6.9 fun iwọn aropin ti aropo
Fun ọkọọkan ti betadex sulfobutyl ether sodium tente oke I–X, wo iwọn opin (% agbegbe tente oke) ni Tabili 7.
Tabili 7

• PH <791>: 4.0-6.8, ninu ojutu 30% (w/v) ninu omi ti ko ni erogba oloro
• Ipinnu OMI, Ọna I <921>: NMT 10.0%
Awọn ibeere afikun
• Iṣakojọpọ ati Ipamọ: Fipamọ sinu awọn apoti ti o ni pipade daradara, ati tọju ni iwọn otutu yara.Dabobo lati ọrinrin.
• AWỌN ỌMỌRỌ: Isami si lati tọkasi lilo rẹ ni iṣelọpọ awọn fọọmu iwọn lilo injectable.
• USP awọn Ilana itọkasi <11>
USP Beta Cyclodextrin RS
USP Betadex Sulfobutyl Eteri iṣuu soda RS
USP Endotoxin RS
USP Sodium kiloraidi RS■1S (NF30)