D-Sorbitol CAS 50-70-4 Assay 97.0 ~ 100.5% Factory High Quality

I-D-Sorbitol (CAS: 50-70-4) EP8.7 Indlela yokuvavanya
D-Glucitol (D-sorbitol).
Umxholo: i-97.0 ipesenti ukuya kwi-102.0 ipesenti (i-anhydrous substance).
ABAlinganiswa
Ukubonakala: umhlophe okanye phantse umhlophe, i-crystalline powder.
Ukunyibilika: Inyibilika kakhulu emanzini, ayinyibiliki kwi-ethanol (96 pesenti).
Ibonisa i-polymorphism (5.9).
UKUCHAZA
Isazisi sokuqala: A.
Isazisi sesibini: B, C, D
A. Phonononga iichromatograms ezifunyenwe kuvavanyo.
Iziphumo: incopho eyintloko kwichromatogram efunyenwe ngesisombululo sovavanyo iyafana nokugcinwa kwexesha kunye nobukhulu kwincopho yenqununu kwichromatogram efunyenwe ngesisombululo sokubhekisela (a).
B. Nyibilikisa i-0.5 g ngokufudumeza kumxube we-0.5 mL ye-pyridine Rand 5 mL ye-acetic anhydride R. Emva kwemizuzu eyi-10 galela isisombululo kwi-25 mL yamanzi eRandi vumela ukuma emanzini anomkhenkce kangangeeyure ezi-2.I-precipitate, i-recrystallised ukusuka kumthamo omncinci we-ethanol (ipesenti ezingama-96) R kwaye yomiswe kwi-vacuo, iyanyibilika (2.2.14) kwi-98℃ ukuya kwi-104℃.
C. Thin-layer chromatography (2.2.27).
Isisombululo sovavanyo.Dissolve i-25 mg yezinto eziza kuhlolwa emanzini R kwaye udibanise kwi-10 mL kunye ne-solvent efanayo.
Isisombululo seReferensi (a).Dissolve i-25 mg ye-sorbitol CRS emanzini R kwaye udibanise kwi-10 mL kunye ne-solvent efanayo.
Isisombululo seReferensi (b).Dissolve 25 mg ye-mannitol CRS kunye ne-25 mg ye-sorbitol CRS emanzini R kwaye udibanise kwi-10 mL kunye ne-solvent efanayo.
Icwecwe: TLC ijeli yesilica G ipleyiti R.
Isigaba seselula: amanzi R, i-ethyl acetate R, ipropanol R (10:20:70V/V/V).
Ukusetyenziswa: 2 μL
Uphuhliso: ngaphezu kwendlela ye-17cm
Ukomisa: emoyeni.
Ukufumanisa: fafaza ngesisombululo se-4-aminobenzoic acid R;yomile kumoya obandayo de i-acetone isuswe;ukushisa kwi-100 ℃ nge-15min;vumela ukupholisa kunye nokutshiza ngesisombululo se-2g / L se-sodium periodate R;yomile kumoya obandayo;shushu kwi-100 ℃ nge-15 min.
Ukufaneleka kwenkqubo: isisombululo sesalathiso (b):
– ikhromatogram ibonisa amabala ama-2 ahlulwe ngokucacileyo.
Iziphumo: indawo ephambili kwichromatogram efunyenwe kunye nesisombululo sovavanyo iyafana kwindawo, umbala kunye nobukhulu kwindawo eyintloko kwichromatogram efunyenwe ngesisombululo sereferensi (a).
D. Ukujikeleza okuthe ngqo kwe-optical (2.2.7): +4.0 ukuya +7.0 (i-anhydrou substance).
Nyibilikisa i-5.00 g yezinto eziza kuhlolwa kunye ne-6.4 g ye-disodium tetraborate R kwi-40 mL yamanzi R. Vumela ukuma i-1h, ukugubha ngamanye amaxesha, kwaye udibanise kwi-50.0mL ngamanzi R. Isihluzo ukuba kuyimfuneko.
UVAVANYO
Ukubonakala kwesisombululo.Isisombululo sicacile (2.2.1) kwaye singenambala (2.2.2, Indlela II).
Dissolve 5 g emanzini R kwaye uhlambulule kwi-50 mL kunye ne-solvent efanayo.
Ukuqhuba (2.2.38): ubuninzi 20 μS·cm−1
Dissolve 20.0 g incarbon dioxide-free water R elungiselelwe kumanzi adibeneyo R kwaye udibanise kwi-100.0 mL kunye ne-solvent efanayo.Ukulinganisa i-conductivity yesisombululo ngelixa uvuselela ngobumnene nge-magnetic stirrer.
Ukunciphisa iishukela: ubuninzi beepesenti ze-0.2, ezichazwe njenge-glucose elinganayo.
Dibanisa i-5.0 g kwi-6 mL yamanzi R ngoncedo lobushushu obuthambileyo.Pholisa kwaye wongeze i-20 mL yesisombululo se-cupri-citric R kunye namaso ambalwa eglasi.Ukushisa ukuze ukubilisa kuqale emva kwemizuzu emi-4 kwaye ugcine ukubilisa i-3 min.Pholisa ngokukhawuleza kwaye wongeze i-100 mL ye-2.4 yepesenti ye-V / V isisombululo se-glacial acetic acid R kunye ne-20.0 mL ye-0.025 M iodine.Ngokushukuma okuqhubekayo, yongeza i-25 mL yomxube we-6 umthamo we-hydrochloric acid R kunye ne-94 umthamo wamanzi R kwaye, xa i-precipitate ichithekile, i-titrate engaphezulu kwe-iodine nge-0.05 M ye-sodium thiosulfate usebenzisa i-1 mL yesisombululo se-starch R, yongezwa. ukuya ekupheleni kwetitration, njengesalathisi.Akukho ngaphantsi kwe-12.8 mL ye-0.05 M ye-sodium thiosulfate iyadingeka.
Izinto ezinxulumeneyo.Ichromatography yolwelo (2.2.29).
Isisombululo sovavanyo.Chitha i-5.0 g yezinto eziza kuhlolwa kwi-20 mL yamanzi R kwaye udibanise kwi-100.0 mL kunye ne-solvent efanayo.
Isisombululo seReferensi (a).Dissolve 0.50g ye-sorbitol CRS kwi-2 mL yamanzi R kwaye udibanise kwi-10.0 mL kunye ne-solvent efanayo.
Isisombululo seReferensi (b).Nciphisa i-2.0mL yesisombululo sovavanyo kwi-100.0 mL ngamanzi R.
Isisombululo seReferensi (c).Nciphisa i-5.0 mL yesisombululo sereferensi (b) ukuya kwi-100.0 mL ngamanzi R.
Isisombululo seReferensi (d).Dissolve 0.5g ye-sorbitol R kunye ne-0.5 g ye-mannitol R (ukungcola A) kwi-5 mL yamanzi R kwaye udibanise kwi-10.0 mL kunye ne-solvent efanayo.
Uluhlu:
–ubungakanani:l=0.3m,Ø=7.8mm
-isigaba sokumisa: i-cation-exchange-resin eqinile (ifom ye-calcium) R (9 μm);
–ubushushu: 85±1°C
Inqanaba elihambayo: Amanzi atshisiweyo R.
Izinga lokuhamba: 0.5mL / min
Ukufunyanwa: irefractometer igcinwe kwiqondo lobushushu elingaguqukiyo (umz. 35 °C).
Isitofu: 20μL yesisombululo sovavanyo kunye nezisombululo zereferensi (b) (c) kunye (d)
Ixesha lokugijima: kabini ixesha lokugcinwa kwe-sorbitol.
Ukugcinwa okuhambelanayo ngokubhekiselele kwi-sorbitol (ixesha lokugcinwa = malunga ne-27 min): ukungcola C = malunga ne-0.6;ukungcola A = malunga ne-0.8;ukungcola B = malunga ne-1.1.
Ukufaneleka kwenkqubo: isisombululo sesalathiso (d):
-isisombululo: ubuncinci be-2.0 phakathi kweencopho ngenxa yokungcola A kunye ne-sorbitol.
Imida:
-nakuphi na ukungcola: kukungcola ngakunye, kungabi ngaphezu kwendawo yencopho yenqununu kwichromatogram efunyenwe ngesisombululo sokubhekisela (b) (2 pesenti);
-itotali: akukho ngaphezu kwe-1.5 amaxesha ommandla wenqununu yenqununu kwi-chromatogram efunyenwe ngesisombululo sokubhekisela (b) (i-3 ekhulwini);
-i-disregard limit: indawo yenqununu yenqununu kwi-chromatogram efunyenwe ngesisombululo sokubhekisela (c) (i-0.1 ekhulwini).
Inkokeli (2.4.10): ubuninzi be-0.5 ppm.
Nickel (2.4.15): ubuninzi 1 ppm.
Nyibilikisa into eza kuvavanywa kwi-150.0 mL yomxube omiselweyo wezinyibilikisi.
Amanzi (2.5.12): ubuninzi beepesenti ze-1.5, kunqunywe kwi-1.00 g.Sebenzisa umxube we-1 ye-formamide R kunye ne-2 imiqulu ye-anhydrous methanol R njenge-solvent.
Usulelo lweMicrobial
Ukuba yenzelwe ukusetyenziswa ekwenzeni amalungiselelo parenteral:
– TAMC: ikhrayitheriya yokwamkela 102CFU / g (2.6.12).
Ukuba ayenzelwanga ukusetyenziswa ekwenzeni amalungiselelo omzali:
– TAMC: ikhrayitheriya yokwamkela 103CFU / g (2.6.12);
– TYMC: inqobo yokwamkelwa 102CFU/g (2.6.12);
-ukungabikho kwe-Escherichia coli (2.6.13);
-ukungabikho kweSalmonella (2.6.13).
I-endotoxins yebhaktheriya (2.6.14).Ukuba yenzelwe ukusetyenziswa ekwenziweni kwamalungiselelo omzali ngaphandle kwenkqubo efanelekileyo yokususa i-endotoxins yebhaktiriya:
- ngaphantsi kwe-4 IU / g kumalungiselelo e-parenteral ene-concentration engaphantsi kwe-100g / L ye-sorbitol
– ngaphantsi kwe-2.5 IU/g kumalungiselelo parenteral abe noxinzelelo lwe-100g/L okanye ngaphezulu kwe-sorbitol
UVAVANYO
I-chromatography yolwelo (2.2.29) njengoko ichaziwe kuvavanyo lwezinto ezinxulumene nolu hlengahlengiso lulandelayo.
Isitofu: isisombululo sovavanyo kunye nesisombululo sereferensi (a).
Bala umxholo wepesenti ye-D-sorbitol ukusuka kumxholo obhengeziweyo we-sorbitol CRS.
LABELING
Ileyibhile ithi:
- apho kufanelekileyo, ubuninzi boxinzelelo lwee-endotoxins zebhaktheriya;
– apho kufanelekileyo, ukuba into ifanelekile ukuba isetyenziswe ekwenzeni amalungiselelo omzali.
UBUNGCOLA
A. D-mannitol,
B. D-iditol,
C. 4-O-α-D-glucopyranosyl-D-glucitol (D-maltitol).

I-D-Sorbitol (i-CAS: 50-70-4) Indlela yoVavanyo lwe-USP
INGCACISO
I-Sorbitol iqulethe i-NLT 91.0% kunye ne-NMT 100.5% ye-D-sorbitol, ibalwe ngokwesiseko se-anhydrous.Izixa zeswekile zizonke, ezinye ii-polyhydric alcohols, kunye naziphi na i-hexitol anhydrides, ukuba zichongiwe, azifakwanga kwiimfuno, okanye kwisixa esibaliweyo phantsi kobunye ubumdaka kwiZaziso eziPhambili.
UKUCHAZA
• A.
Isisombululo sesampuli: 1g yeSorbitol kwi-75 mL yamanzi
Uhlalutyo: Dlulisa i-3 mL yesisombululo seSampule kwi-tube yokuvavanya i-15-cm, kwaye ungeze i-3 mL yesisombululo se-catechol esandula ukulungiswa (1 kwi-10), kwaye udibanise.Yongeza i-6 mL ye-asidi ye-sulfuric, uze ufudumeze ngobunono ityhubhu edangatyeni kangangemizuzu engama-30.
• B. Ixesha lokugcinwa kwencopho enkulu yeSampuli yesisombululo ihambelana nesombululo soMgangatho, njengoko sifunyenwe kuVavanyo.
UVAVANYO
• INKQUBO
Isigaba esiphathwayo: Sebenzisa amanzi athotyiweyo.
Isisombululo sokufaneleka kwenkqubo: Lungiselela isisombululo esiqulethe i-4.8 mg / g ye-USP nganye ye-Sorbitol RS kunye ne-mannitol
Isisombululo esisemgangathweni: 4.8 mg / g ye-USP Sorbitol RS
Isisombululo sesampuli: Dissolve 0.10 g yeSorbitol emanzini, kwaye uhlambulule ngamanzi ukuya kwi-20g.Rekhoda ubunzima bokugqibela besisombululo, kwaye udibanise ngokucokisekileyo.
Inkqubo yeChromatographic
(Jonga iChromatography <621>, Ukufaneleka kweNkqubo.)
Indlela: LC
Umtshina: Isalathiso sokuqhafaza
Ikholamu: 7.8-mm x 10-cm;ukupakisha L34
Ubushushu
Uluhlu: 50±2°
Umtshina: 35 °
Izinga lokuhamba: 0.7 mL / min
Ubungakanani betofu: 10 μL
Ukufaneleka kwenkqubo
Iisampulu: Isisombululo sokufaneleka kwenkqubo kunye nesisombululo esiPhakathi [QAPHELA-Amaxesha okugcinwa kwe-mannitol kunye ne-sorbitol malunga ne-0.6 kunye ne-1.0, ngokulandelanayo.]
Iimfuno zokufaneleka
Isisombululo: I-NLT 2.0 phakathi kwe-sorbitol kunye ne-mannitol, isisombululo sokufaneleka kweNkqubo
Ukutenxa komgangatho ozalanayo: NMT 2.0%, isisombululo esisemgangathweni
Uhlalutyo
Iisampulu: Isisombululo esisemgangathweni kunye nesisombululo seSampuli
Bala ipesenti, ngokwesiseko se-anhydrous, ye-D-sorbitol kwisahlulo seSorbitol esithathiweyo:
Isiphumo = (rU/rS) x (CS/CU) x (100/(100 -W)) x 100
rU= incopho yempendulo evela kuMfanekiso wesisombululo
rS= incopho yempendulo evela kuMgangatho wesisombululo
CS= ukuxinwa kwe-USP Sorbitol RS kwisisombululo esiPhakathi (mg/g)
CU= ukuxinana kweSorbitol kwiSampuli yesisombululo (mg/g)
W= ipesenti efunyenweyo kuvavanyo lokumiselwa kwaManzi
Indlela yokwamkela: 91.0% -100.5% kwisiseko se-anhydrous
UBUNGCOLA
• UMDA UNICKE
Isisombululo sesampuli: Dissolve 20.0 g ye-Sorbitol kwi-acetic acid ehlanjululweyo, kwaye udibanise nge-acetic acid ehlanjululweyo ukuya kwi-150 mL.
Isisombululo esingenanto: 150 mL ye-acetic acid ehlanjululweyo
Izisombululo ezisemgangathweni: Lungiselela izisombululo ezintathu ngokudibanisa i-0.5, 1.0, kunye ne-1.5 mL yesisombululo esiqhelekileyo se-nickel TS ukuya kwi-20.0 g ye-Sorbitol echithwe kwi-acetic acid ehlanjululweyo, kwaye udibanise nge-solvent efanayo kwi-150 mL.
Iimeko zezixhobo
(Jonga iSpectrophotometry kunye nokuSasaza ukukhanya <851>)
Imowudi: Ukufunxa i-atomic spectrophotometry
Ubude bohlalutyo: 232.0 nm
Isibane:Nickel hollow-cathode
Idangatye: Umoya-asetylene
Uhlalutyo
Iisampulu: Izisombululo ezisemgangathweni kunye nesisombululo seSampuli
Kwisampuli nganye yongeza i-2.0 mL yesisombululo se-ammonium pyrrolidinedithiocarbamate egcweleyo (equkethe i-10g / L ye-ammonium pyrrolidinedithiocarbamate) kunye ne-10.0 mL ye-methyl isobutyl ketone, kwaye ugubungele i-30 s.Khusela ekukhanyeni okuqaqambileyo.Vumela iileya ezimbini ukuba zahlukane, kwaye usebenzise i-methyl isobutyl ketone layer.Seta isixhobo siye kuqanda usebenzisa umaleko ophilayo osuka kwisisombululo esingenanto.
Ngokuhambelanayo misela i-absorpension ye-organic layer kwiiSampulu ubuncinane kathathu nganye.Rekhoda umyinge wofundo oluzinzileyo kwizisombululo zoMgangatho ngamnye kunye nesisombululo seSampuli.Phakathi komlinganiselo ngamnye, nqwenela umaleko ophilayo kwisisombululo esingenanto, kwaye uqinisekise ukuba ufundo lubuyela ku-zero.Yenza isicwangciso sokufunxa izisombululo zoMgangatho kunye nesisombululo seSampuli ngokuchasene nesixa esongezelelweyo senikeli.
Yongeza umgca odibanisa amanqaku kwigrafu de idibane ne-axis yoxinaniso.Umgama phakathi kweli nqaku kunye nokudibanisa kwee-axes kubonisa ukuxinwa kwe-nickel kwisisombululo seSample.
Indlela yolwamkelo: NMT 1 ppm
• UKUBULA OKUSISELWEYO <281>: I-NMT 0.1%, imiselwe kwisahlulo se-1.5g
UKUNCIPHA ESWEKILE
[QAPHELA-Imali egqitywe kolu vavanyo ayiqukwanga kwisixa esibaliweyo phantsi kobunye ubumdaka kwiZaziso ngokuBanzi.]
Isisombululo sesampuli: Dibanisa i-3.3 g ye-Sorbitol kwi-3 mL yamanzi ngoncedo lobushushu obuthambileyo.Pholisa, kwaye wongeze i-20.0 mL ye-cupric citrate TS kunye namaso ambalwa eglasi.Ukufudumala ukwenzela ukuba ukubilisa kuqale emva kwemizuzu emi-4, kwaye ugcine ukubilisa i-3 min.Pholisa ngokukhawuleza, kwaye wongeze i-40 mL ye-acetic acid ehlanjululweyo, i-60 mL yamanzi, kunye ne-20.0 mL ye-0.05 ye-iodine VS.Ngokugungqa okuqhubekayo, yongeza i-25 mL yomxube we-6 mL ye-hydrochloric acid kunye ne-94 mL yamanzi.
Uhlalutyo: Xa i-precipitate ichithekile, i-titrate engaphezulu kwe-iodine nge-0.05 N ye-sodium thiosulfate VS usebenzisa i-2mL ye-starch TS, eyongeziweyo ekupheleni kwe-titration, njengesalathisi.
Indlela yokwamkela: i-NLT 12.8 mL ye-0.05 N yesodium thiosulfate VS iyafuneka, ihambelana ne-NMT 0.3% yokunciphisa iswekile, njengeglucose
• I-CHLORIDEAND SULFATE, I-Chloride<221> (ukuba ibhaliwe ukuze isetyenziswe ekulungiseleleni iifomu zedosi yabazali)
Isampulu: 1.5 g
Iinqobo zokwamkela: ISampulu ayibonisi kloridi ngaphezulu kokuhambelana ne-0.10 mL ye-0.020 N hydrochloric acid (NMT 0.0050%).
• CHLORIDEAND SULFATE, Sulfate <221> (ukuba ibhaliwe ukuze isetyenziswe ekulungiseleleni iifomu zedosi yabazali)
Isampulu: 1.0 g
Iinqobo zokwamkelwa: ISampuli ayibonisi ngaphezulu kwesulfate kune-0.10 mL ye-0.020 N sulfuric acid (NMT 0.01%).
IIMVAVANYO EZITHILE
• UVAVANYO LWEMICROBIAL ENUMERATION <61> kunye noVAVANYO LWEMICROORGANISMS ECHAZIWEYO <62>: Ubalo lwe-aerobic lulonke kusetyenziswa i-Plate Method yi-NMT 1000 cfu/g, kunye nenani elidityanisiweyo lokungunda kunye neyeast count yi-NMT 100 cfu/g.
• PH <791>: 3.5-7.0, kwisisombululo se-10% (w / w) kumanzi angenayo i-carbon dioxide
• UKUMISELWA KWAMANZI, Indlela I <921>: NMT 1.5%
CLARITYAND COLOROF SOLUTION(ukuba ileyibheliselwe ukusetyenziswa ekulungiseleleni iifomu zedosi yabazali)
Isampulu: 10.0 g
Uhlalutyo: Nciba iSampulu kwi-100.0 mL yamanzi angenayo i-carbon dioxide.
Indlela yokwamkela: Isisombululo sicacile kwaye asinambala.
• UVAVANYO LWEEENDOTOXIN ZEBHAKteria <85> (ukuba zileyibheliselwe ukusetyenziswa ekulungiseleleni iifomu zedosi yomzali): NMT 4 USP Endotoxin Units/g kwiifom zedosi yabazali ezinoxinzelelo olungaphantsi kwe-100g/L ye-sorbitol, kunye ne-NMT 2.5 USP Endotoxin Units/g kwiifom zedosi ye-parenteral ezine-concentration ye-100g/L okanye ngaphezulu kwe-sorbitol.
IIMFUNO EZONGEZELELWEYO
• UFAKEKILE NOGCINA: Londoloza kwizikhongozeli ezivalwe kakuhle.Akukho mfuneko yokugcina ichaziwe.
• UKUBELISWA: I-Sorbitol elungiselelwe ukusetyenziswa ekulungiseni iifomu zedosi yabazali ibhaliwe.
IMIGANGATHO YE-USP REFERENCE <11>
USP Endotoxin RS
USP Sorbitol RS