D-Sorbitol CAS 50-70-4 Assay 97.0 ~ 100.5% Hoobkas Zoo

D-Sorbitol (CAS: 50-70-4) EP8.7 Test Method
D-Glucitol (D-sorbitol).
Cov ntsiab lus: 97.0 feem pua ​​​​rau 102.0 feem pua ​​(cov khoom tsis muaj dej).
CEEB TOOM
Cov tsos mob: dawb los yog yuav luag dawb, crystalline hmoov.
Solubility: soluble hauv dej heev, xyaum insoluble hauv ethanol (96 feem pua).
Nws qhia txog polymorphism (5.9).
KEV KHO MOB
Kev txheeb xyuas thawj zaug: A.
Kev qhia thib ob: B, C, D
A. Tshawb xyuas cov chromatograms uas tau txais hauv qhov kev xeem.
Cov txiaj ntsig: lub ntsiab lus tseem ceeb hauv chromatogram tau txais nrog cov tshuaj ntsuam xyuas zoo sib xws hauv lub sijhawm khaws cia thiab qhov loj me rau lub ntsiab lus tseem ceeb hauv chromatogram tau nrog kev siv tshuaj (a).
B. Dissolve 0.5 g nrog cua sov nyob rau hauv ib tug sib tov ntawm 0.5 mL ntawm pyridine Rand 5 mL ntawm acetic anhydride R. Tom qab 10 min ncuav lub tov rau hauv 25 mL ntawm dej Rand cia sawv ntsug nyob rau hauv dej txias rau 2 h.Lub precipitate, recrystallised los ntawm ib tug me me ntim ntawm ethanol (96 ib xees) R thiab qhuav nyob rau hauv vacuo, melts (2.2.14) ntawm 98 ℃ to 104 ℃.
C. Nyias-txheej chromatography (2.2.27).
Test daws.Dissolve 25 mg ntawm cov tshuaj yuav tsum tau soj ntsuam nyob rau hauv dej R thiab dilute mus rau 10 mL nrog tib hnyav.
Kev daws teeb meem (a).Dissolve 25 mg ntawm sorbitol CRS hauv dej R thiab dilute mus rau 10 mL nrog tib cov kuab tshuaj.
Kev daws teeb meem (b).Dissolve 25 mg ntawm mannitol CRS thiab 25 mg ntawm sorbitol CRS hauv dej R thiab dilute mus rau 10 mL nrog tib cov kuab tshuaj.
Phaj: TLC silica gel G phaj R.
Mobile theem: dej R, ethyl acetate R, propanol R (10: 20: 70V / V / V).
Daim ntawv thov: 2 μL
Kev loj hlob: tshaj ib txoj kev ntawm 17cm
Qhuav: hauv huab cua.
Kev kuaj pom: tshuaj tsuag nrog 4-aminobenzoic acid tov R;qhuav nyob rau hauv ib tug tam sim no ntawm huab cua txias kom txog thaum lub acetone tshem tawm;kub ntawm 100 ℃ rau 15 min;cia txias thiab tshuaj tsuag nrog 2g / L tov ntawm sodium periodate R;qhuav nyob rau hauv ib tug tam sim no ntawm huab cua txias;Kub ntawm 100 ℃ rau 15 min.
System suitability: reference solution (b):
- cov chromatogram qhia 2 qhov sib cais kom meej.
Cov txiaj ntsig: qhov chaw tseem ceeb hauv chromatogram tau txais nrog cov tshuaj ntsuam xyuas zoo sib xws hauv txoj hauj lwm, xim thiab qhov loj me rau qhov chaw tseem ceeb hauv chromatogram tau nrog kev siv tshuaj (a).
D. Kev sib hloov kho qhov muag tshwj xeeb (2.2.7): +4.0 txog +7.0 (anhydrou tshuaj).
Dissolve 5.00 g ntawm cov tshuaj yuav tsum tau soj ntsuam thiab 6.4 g ntawm disodium tetraborate R nyob rau hauv 40 mL dej R. Cia sawv ntsug rau 1h, co qee zaus, thiab dilute mus rau 50.0mL nrog dej R. Lim yog tsim nyog.
KEV KAWM
Qhov tshwm sim ntawm kev daws.Qhov kev daws teeb meem yog qhov tseeb (2.2.1) thiab tsis muaj xim (2.2.2, Txoj Kev II).
Dissolve 5 g hauv dej R thiab dilute mus rau 50 mL nrog tib cov kuab tshuaj.
Conductivity (2.2.38): siab tshaj 20 μS·cm−1
Dissolve 20.0 g incarbon dioxide-dawb dej R npaj los ntawm distilled dej R thiab dilute mus rau 100.0 mL nrog tib hnyav.Ntsuas cov conductivity ntawm cov tshuaj thaum maj mam nplawm nrog ib tug sib nqus stirrer.
Txo cov suab thaj: siab tshaj 0.2 feem pua, qhia tias yog cov piam thaj sib npaug.
Dissolve 5.0 g hauv 6 mL dej R nrog kev pab ntawm maj mam tshav kub.Txias thiab ntxiv 20 mL ntawm cupri-citric tov R thiab ob peb iav hlaws dai.Tshav kub kom npau npau pib tom qab 4 feeb thiab tuav lub boil rau 3 feeb.Txias sai sai thiab ntxiv 100 mL ntawm 2.4 feem pua ​​​​V / V tov ntawm glacial acetic acid R thiab 20.0 mL ntawm 0.025 M iodine.Nrog tas li co, ntxiv 25 mL ntawm ib tug sib tov ntawm 6 ntim ntawm hydrochloric acid R thiab 94 ntim dej R thiab, thaum lub precipitate tau yaj, titrate tshaj ntawm iodine nrog 0.05 M sodium thiosulfate siv 1 mL ntawm starch tov R, ntxiv. mus rau qhov kawg ntawm titration, raws li qhov taw qhia.Yuav tsum tsis pub tsawg tshaj 12.8 mL ntawm 0.05 M sodium thiosulfate.
Cov khoom muaj feem xyuam.Ua kua chromatography (2.2.29).
Test daws.Dissolve 5.0 g ntawm cov tshuaj yuav tsum tau kuaj nyob rau hauv 20 mL dej R thiab dilute mus rau 100.0 mL nrog tib hnyav.
Kev daws teeb meem (a).Dissolve 0.50g ntawm sorbitol CRS hauv 2 mL dej R thiab dilute mus rau 10.0 mL nrog tib cov kuab tshuaj.
Kev daws teeb meem (b).Dilute 2.0mL ntawm cov tshuaj ntsuam xyuas rau 100.0 mL nrog dej R.
Kev daws teeb meem (c).Dilute 5.0 mL ntawm kev siv tshuaj (b) rau 100.0 mL nrog dej R.
Kev daws teeb meem (d).Dissolve 0.5g ntawm sorbitol R thiab 0.5 g ntawm mannitol R ( impurity A) hauv 5 mL dej R thiab dilute mus rau 10.0 mL nrog tib cov kuab tshuaj.
Kem:
Luas = 0.3 m, Ø 7.8 mm
-stationary theem: muaj zog cation-exchange resin (calcium form) R (9 μm);
Qhov kub thiab txias: 85 ± 1 ° C
Mobile theem: degassed dej R.
Tus nqi ntws: 0.5mL / min
Kev kuaj pom: refractometer khaws cia ntawm qhov kub thiab txias (piv txwv li 35 ° C).
Txhaj tshuaj: 20μL ntawm cov tshuaj ntsuam xyuas thiab siv cov kev daws teeb meem (b) (c) thiab (d)
Lub sijhawm ua haujlwm: ob zaug lub sijhawm khaws cia ntawm sorbitol.
Cov txheeb ze tuav nrog siv sorbitol (lub sijhawm khaws cia = txog 27 min): impurity C = txog 0.6;impurity A = txog 0.8;impurity B = txog 1.1.
System suitability: reference solution (d):
-kev daws teeb meem: yam tsawg kawg 2.0 nruab nrab ntawm lub ncov vim impurity A thiab sorbitol.
txwv:
-Txhua yam impurity: rau txhua qhov impurity, tsis pub ntau tshaj qhov chaw ntawm lub hauv paus ncov hauv chromatogram tau nrog kev siv tshuaj (b) (2 feem pua);
-tag nrho: tsis pub ntau tshaj 1.5 npaug ntawm thaj tsam ntawm lub hauv paus ncov hauv chromatogram tau nrog kev siv tshuaj (b) (3 feem pua);
-tsis quav ntsej txwv: thaj tsam ntawm lub hauv paus ncov hauv chromatogram tau txais nrog kev siv tshuaj (c) (0.1 feem pua).
Lead (2.4.10): siab tshaj 0.5ppm.
Nickel (2.4.15): siab tshaj 1 ppm.
Dissolve cov tshuaj yuav tsum tau kuaj nyob rau hauv 150.0 mL ntawm cov tshuaj sib tov ntawm cov kuab tshuaj.
Dej (2.5.12): siab tshaj 1.5 feem pua, txiav txim siab ntawm 1.00 g.Siv ib qho sib xyaw ntawm 1 ntim ntawm formamide R thiab 2 ntim ntawm anhydrous methanol R ua hnyav.
Cov kab mob microbial
Yog hais tias npaj rau siv nyob rau hauv kev tsim cov parenteral npaj:
- TAMC: kev lees paub 102CFU/g (2.6.12).
Yog tias tsis npaj rau kev siv hauv kev tsim cov tshuaj parenteral:
- TAMC: kev lees paub 103CFU/g (2.6.12);
- TYMC: kev lees paub 102CFU/g (2.6.12);
- tsis muaj Escherichia coli (2.6.13);
- tsis muaj Salmonella (2.6.13).
Cov kab mob endotoxins (2.6.14).Yog tias npaj rau kev siv hauv kev tsim cov tshuaj parenteral yam tsis muaj cov txheej txheem ntxiv tsim nyog rau kev tshem tawm cov kab mob endotoxins:
- tsawg dua 4 IU / g rau kev npaj parenteral uas muaj cov ntsiab lus tsawg dua 100g / L ntawm sorbitol
- tsawg dua 2.5 IU / g rau kev npaj parenteral uas muaj cov ntsiab lus ntawm 100g / L lossis ntau dua ntawm sorbitol
QHIA
Liquid chromatography (2.2.29) raws li tau piav qhia hauv kev sim rau cov tshuaj muaj feem xyuam nrog kev hloov kho hauv qab no.
Txhaj tshuaj: kuaj tshuaj thiab siv tshuaj (a).
Xam cov ntsiab lus feem pua ​​​​ntawm D-sorbitol los ntawm cov ntsiab lus tshaj tawm ntawm sorbitol CRS.
LABELING
Daim ntawv lo hais tias:
- qhov twg siv tau, qhov siab tshaj plaws ntawm cov kab mob endotoxins;
- qhov muaj feem xyuam, cov khoom tsim nyog rau kev siv cov khoom siv parenteral npaj.
IMPURITIES
A. D-mannitol,
B. D-iditol,
C. 4-O-α-D-glucopyranosyl-D-glucitol (D-maltitol).

D-Sorbitol (CAS: 50-70-4) USP Test Method
DEFINITION
Sorbitol muaj NLT 91.0% thiab NMT 100.5% ntawm D-sorbitol, suav nrog lub hauv paus anhydrous.Tus nqi ntawm tag nrho cov suab thaj, lwm yam dej cawv polyhydric, thiab ib qho hexitol anhydrides, yog tias kuaj pom, tsis suav nrog hauv cov kev xav tau, lossis nyob rau hauv tus lej suav raws li Lwm Cov Khoom Siv Hauv Cov Ntawv Ceeb Toom.
IDENTIFICATION
• A.
Piv txwv li: 1g ntawm Sorbitol hauv 75 mL dej
Kev tsom xam: Hloov 3 mL ntawm cov qauv tshuaj mus rau lub raj 15-cm, thiab ntxiv 3 mL ntawm cov tshuaj catechol tshiab (1 hauv 10), thiab sib tov.Ntxiv 6 mL ntawm sulfuric acid, maj mam muab tso rau hauv lub qhov cub rau 30 feeb.
• B. Lub sij hawm tuav ntawm lub ncov loj ntawm cov qauv kev daws teeb meem sib raug rau qhov ntawd los ntawm cov txheej txheem kev daws teeb meem, raws li tau txais hauv Assay.
QHIA
• KEV PAB CUAM
Mobile theem: Siv dej degassed.
Kev daws teeb meem tsim nyog: Npaj cov tshuaj uas muaj 4.8 mg / g ntawm txhua USP Sorbitol RS thiab mannitol
Kev daws teeb meem: 4.8 mg / g ntawm USP Sorbitol RS
Piv txwv li: Dissolve 0.10 g ntawm Sorbitol hauv dej, thiab dilute nrog dej mus rau 20g.Sau qhov kawg daws qhov hnyav, thiab sib tov kom huv si.
Chromatographic system
(Saib Chromatography <621>, System Suitability.)
Qauv: LC
Detector: Refractive Index
Kem: 7.8-mm x 10-cm;kev L34
Kub
Kem: 50 ± 2 °
Ntes: 35 °
Tus nqi ntws: 0.7 mL / min
Kev txhaj tshuaj loj: 10 μL
Qhov system haum
Cov Qauv: Cov kev daws teeb meem tsim nyog thiab cov qauv kev daws teeb meem [CEEB TOOM-Lub sij hawm tuav cov txheeb ze rau mannitol thiab sorbitol yog kwv yees li 0.6 thiab 1.0, feem.]
Suitability xav tau
Kev daws teeb meem: NLT 2.0 ntawm sorbitol thiab mannitol, Kev daws teeb meem tsim nyog
Tus txheeb ze tus qauv sib txawv: NMT 2.0%, Standard tov
Kev tsom xam
Qauv: Cov qauv kev daws teeb meem thiab cov qauv kev daws teeb meem
Xam cov feem pua, ntawm lub hauv paus anhydrous, ntawm D-sorbitol nyob rau hauv ib feem ntawm Sorbitol noj:
Result = (rU/rS) x (CS/CU) x (100/(100 -W)) x 100
rU = ncov teb los ntawm Sample tov
rS = ncov teb los ntawm Standard tov
CS = concentration ntawm USP Sorbitol RS nyob rau hauv Standard tov (mg / g)
CU = concentration ntawm Sorbitol nyob rau hauv cov qauv tov (mg / g)
W = feem pua ​​​​tau txais hauv kev xeem rau Kev Txiav Txim Dej
Kev lees txais cov qauv: 91.0% -100.5% ntawm lub hauv paus anhydrous
IMPURITIES
• LIMITOF NICKE
Piv txwv li: Dissolve 20.0 g ntawm Sorbitol nyob rau hauv diluted acetic acid, thiab diluted nrog diluted acetic acid rau 150 mL.
Cov tshuaj dawb: 150 mL ntawm diluted acetic acid
Cov txheej txheem kev daws teeb meem: Npaj peb txoj kev daws teeb meem los ntawm kev ntxiv 0.5, 1.0, thiab 1.5 mL ntawm nickel standard tov TS rau 20.0 g ntawm Sorbitol yaj hauv diluted acetic acid, thiab dilute nrog tib cov kuab tshuaj rau 150 mL.
Instrumental mob
(Saib Spectrophotometry thiab Lub Teeb-Scattering <851>)
Hom: Atomic absorption spectrophotometric
Kev ntsuas wavelength: 232.0nm
Lub teeb: Nickel hollow-cathode
Nplaim: Cua-acetylene
Kev tsom xam
Qauv: Cov qauv kev daws teeb meem thiab cov qauv kev daws teeb meem
Rau txhua tus qauv ntxiv 2.0 mL ntawm saturated ammonium pyrrolidinedithiocarbamate tov (muaj 10g / L ntawm ammonium pyrrolidinedithiocarbamate) thiab 10.0 mL ntawm methyl isobutyl ketone, thiab co rau 30 s.Tiv thaiv los ntawm lub teeb ci.Cia ob txheej sib cais, thiab siv cov txheej txheem methyl isobutyl ketone.Teem lub ntsuas rau xoom siv cov organic txheej los ntawm Blank tov.
Concomitantly txiav txim siab absorbances ntawm cov organic txheej los ntawm cov qauv tsawg kawg peb zaug txhua.Sau qhov nruab nrab ntawm cov ntawv nyeem tsis tu ncua rau txhua qhov kev daws teeb meem Standard thiab cov qauv kev daws teeb meem.Nruab nrab ntawm txhua qhov kev ntsuas, aspirate cov organic txheej los ntawm Blank tov, thiab paub tseeb tias qhov kev nyeem ntawv rov qab mus rau xoom.Npaj cov absorbances ntawm Standard daws teeb meem thiab cov qauv tov piv rau ntxiv kom muaj nuj nqis ntawm npib tsib xee.
Extrapolate kab koom nrog cov ntsiab lus ntawm daim duab kom txog rau thaum nws ua tau raws li qhov concentration axis.Qhov kev ncua deb ntawm qhov taw tes no thiab kev sib tshuam ntawm cov axes sawv cev rau qhov concentration ntawm npib tsib xee hauv cov qauv tshuaj.
Kev lees txais: NMT 1 ppm
• RESIDUEON IGNITION <281>: NMT 0.1%, txiav txim siab ntawm 1.5g feem
QHOV TSEEB
[CEEB TOOM-Tus nqi txiav txim siab hauv qhov kev sim no tsis suav nrog hauv cov nyiaj suav nrog hauv Lwm Cov Khoom Siv Hauv Cov Ntawv Ceeb Toom.]
Piv txwv li: Dissolve 3.3 g ntawm Sorbitol hauv 3 mL dej nrog kev pab ntawm maj mam tshav kub.Txias, thiab ntxiv 20.0 mL ntawm khob citrate TS thiab ob peb iav hlaws dai.Tshav kub kom npau npau pib tom qab 4 feeb, thiab tuav lub boil rau 3 feeb.Txias sai sai, thiab ntxiv 40 mL ntawm diluted acetic acid, 60 mL dej, thiab 20.0 mL ntawm 0.05 N iodine VS.Nrog tas li co, ntxiv 25 mL ntawm ib tug sib tov ntawm 6 mL ntawm hydrochloric acid thiab 94 mL dej.
Kev tsom xam: Thaum cov dej nag tau yaj, titrate ntau tshaj ntawm iodine nrog 0.05 N sodium thiosulfate VS siv 2mL ntawm cov hmoov txhuv nplej siab TS, ntxiv rau qhov kawg ntawm titration, raws li qhov taw qhia.
Kev lees txais: NLT 12.8 mL ntawm 0.05 N sodium thiosulfate VS yog xav tau, sib xws rau NMT 0.3% ntawm kev txo cov suab thaj, raws li cov piam thaj.
• CHLORIDEAND SULFATE, Chloride <221> (yog tias sau npe siv rau hauv kev npaj cov ntawv noj tshuaj parenteral)
Qauv: 1.5 g
Kev lees txais cov qauv: Cov qauv qhia tsis muaj cov tshuaj chloride ntau dua li 0.10 mL ntawm 0.020 N hydrochloric acid (NMT 0.0050%).
• CHLORIDEAND SULFATE, Sulfate <221> (yog tias tau sau npe siv rau hauv kev npaj cov ntawv noj tshuaj parenteral)
Qauv: 1.0g
Kev lees txais cov qauv: Cov qauv qhia tsis muaj sulfate ntau dua li 0.10 mL ntawm 0.020 N sulfuric acid (NMT 0.01%).
TSEEM CEEB
• MICROBIAL ENUMERATION TESTS <61> thiab TESTS FOR SPECIFIED MICROORGANISMS <62>: Tag nrho cov suav aerobic siv Plate Method yog NMT 1000 cfu/g, thiab tag nrho cov pwm thiab cov poov xab suav suav yog NMT 100 cfu/g
• PH <791>: 3.5-7.0, hauv 10% (w/w) tov hauv dej tsis muaj carbon dioxide
• KEV TIV THAIV DUA, Txoj Kev I <921>: NMT 1.5%
CLARITYAND COLOROF SOLUTION (yog tias sau npe rau kev siv hauv kev npaj cov ntawv noj tshuaj parenteral)
Qhov hnyav: 10.0 g
Kev Ntsuam Xyuas: Dissolve cov qauv hauv 100.0 mL ntawm cov dej tsis muaj carbon dioxide.
Kev lees txais cov qauv: Cov tshuaj yog ntshiab thiab tsis muaj xim.
• BACTERIAL ENDOTOXINS TEST <85> (yog tias sau npe rau siv hauv kev npaj cov ntawv noj tshuaj parenteral): NMT 4 USP Endotoxin Units/g rau parenteral dosage forms uas muaj ntau dua 100g/L ntawm sorbitol, thiab NMT 2.5 USP Endotoxin Units/g rau cov ntaub ntawv parenteral ntau npaum li cas muaj qhov concentration ntawm 100g / L lossis ntau dua ntawm sorbitol.
TSEEM CEEB
• PACKAGINGAND STORAGE: Khaws rau hauv cov thawv kaw kom zoo.Tsis muaj qhov yuav tsum tau khaws cia.
• LABELING: Sorbitol npaj los siv rau hauv kev npaj cov ntaub ntawv noj tshuaj parenteral yog li sau npe.
USP REFERENCE STANDARDS <11>
Tom ntej: USP Endotoxin RS
USP Sorbitol RS