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

D-Sorbitol (CAS: 50-70-4) EP8.7 Njira Yoyesera
D-Glucitol (D-sorbitol).
Zomwe zili: 97.0% mpaka 102.0% (anhydrous substance).
AKALE
Maonekedwe: woyera kapena pafupifupi woyera, crystalline ufa.
Kusungunuka: kusungunuka kwambiri m'madzi, pafupifupi kosasungunuka mu Mowa (96 peresenti).
Ikuwonetsa polymorphism (5.9).
DENTIFICATION
Chidziwitso choyamba: A.
Chizindikiritso Chachiwiri: B, C, D
A. Yang'anani ma chromatogram omwe apezeka pakuyesa.
Zotsatira: pachimake pachimake pa chromatogram yomwe idapezedwa ndi yankho la mayeso ndi yofanana ndi nthawi yosungira komanso kukula kwake ndi pachimake pa chromatogram yopezedwa ndi yankho lolozera (a).
B. Sungunulani 0,5 g ndi kutentha mu chisakanizo cha 0.5 mL wa pyridine Rand 5 mL wa acetic anhydride R. Pakatha mphindi 10, tsanulirani yankho mu 25 mL ya madzi Randi lolani kuyima m'madzi oundana kwa 2 h.The precipitate, recrystallised kuchokera ku voliyumu yaing'ono ya ethanol (96 peresenti) R ndi zouma mu vacuo, zimasungunuka (2.2.14) pa 98 ℃ mpaka 104 ℃.
C. Thin-wosanjikiza chromatography (2.2.27).
Njira yothetsera mayeso.Sungunulani 25 mg wa mankhwala kuti afufuzidwe m'madzi R ndi kuchepetsa 10 mL ndi zosungunulira zomwezo.
Yankho lolozera (a).Sungunulani 25 mg wa sorbitol CRS m'madzi R ndi kuchepetsa 10 mL ndi zosungunulira zomwezo.
Yankho lolozera (b).Sungunulani 25 mg wa mannitol CRS ndi 25 mg wa sorbitol CRS m'madzi R ndi kuchepetsa 10 mL ndi zosungunulira zomwezo.
Plate: TLC silika gel G mbale R.
Gawo la mafoni: madzi R, ethyl acetate R, propanol R (10:20:70V/V/V).
Kugwiritsa ntchito: 2 μL
Kukula: pamtunda wa 17cm
Kuyanika: mumlengalenga.
Kuzindikira: utsi ndi 4-aminobenzoic asidi njira R;kuuma mu mpweya wozizira mpaka acetone itachotsedwa;kutentha kwa 100 ℃ kwa mphindi 15;kulola kuziziritsa ndi kupopera mankhwala ndi 2g/L yankho la sodium periodate R;youma mu mpweya wozizira;kutentha kwa 100 ℃ kwa mphindi 15.
Kuyenerera kwadongosolo: yankho lolozera (b):
- chromatogram imawonetsa mawanga awiri olekanitsidwa bwino.
Zotsatira: malo ofunikira mu chromatogram yopezedwa ndi yankho la mayeso ndi ofanana ndi malo, mtundu ndi kukula kwa malo oyambira mu chromatogram yopezedwa ndi yankho lolozera (a).
D. Kusintha kwapadera kwa kuwala (2.2.7): +4.0 mpaka +7.0 (anhydrou substance).
Sungunulani 5.00 g ya chinthu chomwe chiyenera kuyesedwa ndi 6.4 g ya disodium tetraborate R mu 40 mL ya madzi R. Lolani kuyima kwa 1h, kugwedezeka nthawi zina, ndi kuchepetsa ku 50.0mL ndi madzi R. Sefa ngati kuli kofunikira.
MAYESO
Maonekedwe a yankho. Njira yothetsera vutoli ndi yomveka (2.2.1) komanso yopanda mtundu (2.2.2, Njira II).
Sungunulani 5 g m'madzi R ndi kuchepetsa 50 mL ndi zosungunulira zomwezo.
Conductivity (2.2.38): pazipita 20 μS · cm−1
Sungunulani 20.0 g madzi opanda carbon dioxide R okonzedwa kuchokera ku madzi osungunuka R ndi kuchepetsa 100.0 mL ndi zosungunulira zomwezo.Yezerani kuchuluka kwa yankho ndikuyambitsa mofatsa ndi maginito oyambitsa.
Kuchepetsa shuga: pazipita 0,2 peresenti, yowonetsedwa ngati glucose wofanana.
Sungunulani 5.0 g mu 6 mL madzi R ndi chithandizo cha kutentha pang'ono.Kuziziritsa ndi kuwonjezera 20 mL wa cupri-citric solution R ndi mikanda yagalasi yochepa.Kutenthetsa kuti kuwira kuyambike pambuyo pa 4 min ndikuphika kwa mphindi zitatu.Kuziziritsa msanga ndi kuwonjezera 100 mL ya 2.4 peresenti V/V njira ya glacial acetic acid R ndi 20.0 mL ya 0.025 M ayodini.Ndi kugwedezeka kosalekeza, onjezerani 25 ml ya osakaniza 6 voliyumu ya hydrochloric acid R ndi 94 voliyumu ya madzi R ndipo, mpweya ukasungunuka, tsitsani ayodini wochuluka ndi 0.05 M sodium thiosulfate pogwiritsa ntchito 1 mL ya wowuma njira R, anawonjezera. kumapeto kwa titration, monga chizindikiro.Osachepera 12.8 mL wa 0.05 M sodium thiosulfate amafunikira.
Zogwirizana nazo.Chromatography yamadzimadzi (2.2.29).
Njira yothetsera mayeso.Sungunulani 5.0 g wa chinthu chomwe chiyenera kuyesedwa mu 20 ml ya madzi R ndi kuchepetsa 100.0 mL ndi zosungunulira zomwezo.
Yankho lolozera (a).Sungunulani 0,50g ya sorbitol CRS mu 2 mL ya madzi R ndi kuchepetsa 10.0 mL ndi zosungunulira zomwezo.
Yankho lolozera (b).Sungunulani 2.0mL ya njira yoyesera ku 100.0 mL ndi madzi R.
Yankho lolozera (c).Sungunulani 5.0 mL ya njira yothetsera (b) mpaka 100.0 mL ndi madzi R.
Yankho lolozera (d).Sungunulani 0,5g ya sorbitol R ndi 0,5 g ya mannitol R (chidetso A) mu 5 ml ya madzi R ndi kuchepetsa 10.0 mL ndi zosungunulira zomwezo.
Mzere:
-kukula:l=0.3m,Ø=7.8mm
-ima gawo: amphamvu cation-kusinthanitsa utomoni (calcium mawonekedwe) R (9 μm);
-Kutentha: 85±1°C
Mobile gawo: degassed water R.
Kuthamanga: 0.5mL / min
Kuzindikira: refractometer imasungidwa kutentha kosasintha (mwachitsanzo 35 ° C).
Jekeseni: 20μL ya yankho la mayeso ndi mayankho (b) (c) ndi (d)
Nthawi yothamanga: kawiri nthawi yosungira sorbitol.
Kusungidwa kwachibale ponena za sorbitol (nthawi yosungira = pafupifupi 27 min): zonyansa C = pafupifupi 0.6;chodetsedwa A = pafupifupi 0,8;Chidetso B = pafupifupi 1.1.
Kuyenerera kwamakina: yankho lolozera (d):
-kusamvana: osachepera 2.0 pakati pa nsonga chifukwa cha zodetsa A ndi sorbitol.
Malire:
-chidetso chilichonse: pa chodetsa chilichonse, osapitilira gawo la pachimake chachikulu mu chromatogram yomwe idapezedwa ndi yankho lolozera (b) (2 peresenti);
-chiwerengero: osapitilira nthawi 1.5 gawo la pachimake chachikulu mu chromatogram yopezedwa ndi yankho lolozera (b) (3 peresenti);
-kunyalanyaza malire: gawo lachiwongola dzanja chachikulu mu chromatogram yopezedwa ndi yankho lachidziwitso (c) (0.1 peresenti).
Kutsogolera (2.4.10): pazipita 0.5 ppm.
Nickel (2.4.15): pazipita 1 ppm.
Sungunulani chinthucho kuti chiwunikidwe mu 150.0 ml ya mankhwala osakaniza osakaniza.
Madzi (2.5.12): pazipita 1.5 peresenti, anatsimikiza pa 1.00 g.Gwiritsani ntchito kusakaniza kwa 1 voliyumu ya formamide R ndi ma voliyumu 2 a anhydrous methanol R monga zosungunulira.
Kuwonongeka kwa tizilombo
Ngati agwiritsidwa ntchito popanga zokonzekera za parenteral:
- TAMC: muyezo wovomerezeka 102CFU/g (2.6.12).
Ngati sichinapangidwe kuti chigwiritsidwe ntchito popanga zokonzekera za parenteral:
- TAMC: muyezo wovomerezeka 103CFU/g (2.6.12);
- TYMC: muyezo wovomerezeka 102CFU/g (2.6.12);
-kusowa kwa Escherichia coli (2.6.13);
-kusowa kwa Salmonella (2.6.13).
Mabakiteriya endotoxins (2.6.14).Ngati agwiritsidwa ntchito popanga zokonzekera za makolo popanda njira ina yoyenera yochotsera ma endotoxins a bakiteriya:
- zosakwana 4 IU/g kwa parenteral kukonzekera ndi ndende zosakwana 100g/L wa sorbitol;
- zosakwana 2.5 IU/g kwa parenteral kukonzekera ndi ndende ya 100g/L kapena kuposa sorbitol
ZOYESA
Liquid chromatography (2.2.29) monga momwe tafotokozera poyesa zinthu zokhudzana ndi zosintha zotsatirazi.
Jekeseni: yankho loyesa ndi yankho lolozera (a).
Kuwerengera kuchuluka kwa D-sorbitol kuchokera ku sorbitol CRS yomwe yalengezedwa.
LABELING
Lembalo limati:
- ngati kuli koyenera, kuchuluka kwambiri kwa ma endotoxins a bakiteriya;
- ngati kuli koyenera, kuti chinthucho ndi choyenera kugwiritsidwa ntchito popanga zokonzekera za parenteral.
ZOCHITSA
A. D-mannitol,
B. D-iditol,
C. 4-O-α-D-glucopyranosyl-D-glucitol (D-maltitol).

D-Sorbitol (CAS: 50-70-4) Njira Yoyesera ya USP
TANTHAUZO
Sorbitol ili ndi NLT 91.0% ndi NMT 100.5% ya D-sorbitol, yowerengedwa pa maziko a anhydrous.Kuchuluka kwa mashuga okwana, ma alcohols ena a polyhydric, ndi hexitol anhydrides aliwonse, ngati apezeka, sakuphatikizidwa muzofunikira, kapena kuchuluka kowerengedwa pansi pa Zonyansa Zina mu Zidziwitso Zonse.
CHIZINDIKIRO
• A.
Yankho lachitsanzo: 1g ya Sorbitol mu 75 ml ya madzi
Kuwunika: Tumizani 3 ml ya yankho lachitsanzo mu chubu choyesera cha 15-cm, ndikuwonjezera 3 ml ya yankho la catechol (1 pa 10), ndikusakaniza.Onjezerani 6 mL wa sulfuric acid, kenaka tenthetsani chubu pamoto kwa 30 s.
• B. Nthawi yosungitsa pachimake chachikulu cha Sample solution ikufanana ndi yomwe yachokera mu Standard solution, monga momwe zapezedwa mu Assay.
ZOYESA
• NTCHITO
Gawo la mafoni: Gwiritsani ntchito madzi osungunuka.
Njira yothetsera kuyenerera: Konzani yankho lomwe lili ndi 4.8 mg/g ya USP iliyonse ya Sorbitol RS ndi mannitol
Njira yothetsera: 4.8 mg/g ya USP Sorbitol RS
Yankho lachitsanzo: Sungunulani 0,10 g wa Sorbitol m'madzi, ndi kusungunula ndi madzi mpaka 20g.Lembani kulemera kwa yankho lomaliza, ndikusakaniza bwino.
Chromatographic system
(Onani Chromatography <621>, Kukwanira Kwadongosolo.)
Njira: LC
Detector: Refractive index
Mzere: 7.8-mm x 10-cm;kunyamula L34
Kutentha
Mzere: 50±2°
Chowunikira: 35 °
Kuthamanga: 0.7 mL / min
Kukula kwa jekeseni: 10 μL
Kuyenerera kwadongosolo
Zitsanzo: Njira yothetsera kuyenerera kwadongosolo ndi njira yokhazikika [Dziwani-Nthawi zosungirako za mannitol ndi sorbitol ndi pafupifupi 0.6 ndi 1.0, motsatana.]
Zofunikira zoyenera
Kusamvana: NLT 2.0 pakati pa sorbitol ndi mannitol, Njira yothetsera kuyenerera
Kupatuka kofananira: NMT 2.0%, njira yokhazikika
Kusanthula
Zitsanzo: Yankho lokhazikika ndi yankho lachitsanzo
Kuwerengera kuchuluka, pamaziko a anhydrous, a D-sorbitol mu gawo la Sorbitol yotengedwa:
Zotsatira = (rU/rS) x (CS/CU) x (100/(100 -W)) x 100
rU= nsonga ya yankho lachitsanzo
rS= kuyankha kwakukulu kuchokera ku Standard solution
CS= kuchuluka kwa USP Sorbitol RS mu Standard solution (mg/g)
CU = kuchuluka kwa Sorbitol mu Sample solution (mg/g)
W = peresenti yomwe idapezedwa poyesa Kutsimikiza kwa Madzi
Njira zolandirira: 91.0% -100.5% pamaziko a anhydrous
ZOCHITSA
• LIMITOF NICKE
Yankho lachitsanzo: Sungunulani 20.0 g wa Sorbitol mu asidi acetic wosungunuka, ndi kusungunula ndi asidi acetic wochepetsedwa kufika 150 ml.
Njira yopanda kanthu: 150 mL ya asidi acetic wochepetsedwa
Standard zothetsera: Konzani njira zitatu powonjezera 0,5, 1.0, ndi 1.5 mL ya nickel standard solution TS ku 20.0 g ya Sorbitol yosungunuka mu asidi acetic acid, ndi kusungunula ndi zosungunulira zomwezo ku 150 ml.
Zida zoimbira
(Onani Spectrophotometry and Light-Scattering <851>)
Njira: Atomic mayamwidwe spectrophotometry
Kutalika kwa mafunde: 232.0 nm
Nyali: Nickel hollow-cathode
Lawi lamoto: Air-acetylene
Kusanthula
Zitsanzo: Mayankho okhazikika ndi mayankho achitsanzo
Pachitsanzo chilichonse onjezerani 2.0 mL ya saturated ammonium pyrrolidinedithiocarbamate solution (yokhala ndi 10g/L ya ammonium pyrrolidinedithiocarbamate) ndi 10.0 mL ya methyl isobutyl ketone, ndikugwedezani kwa 30 s.Tetezani ku kuwala kowala.Lolani zigawo ziwirizo kuti zilekanitse, ndipo gwiritsani ntchito methyl isobutyl ketone layer.Khazikitsani chida kukhala ziro pogwiritsa ntchito wosanjikiza wa organic kuchokera mu njira yopanda kanthu.
Nthawi yomweyo dziwani kuyamwa kwa organic wosanjikiza kuchokera ku Zitsanzo zosachepera katatu iliyonse.Lembani avareji ya kuwerengeka kosasunthika pa yankho lililonse la Standard ndi yankho la Zitsanzo.Pakati pa muyeso uliwonse, funani organic wosanjikiza kuchokera mu Chopanda Chopanda yankho, ndikuwonetsetsa kuti kuwerengako kumabwerera ku ziro.Ganizirani momwe mungayankhire mayankho a Standard Solutions ndi Sample solution motsutsana ndi kuchuluka kwa faifi tambala.
Onjezani mzere wolumikizana ndi mfundo pa graph mpaka utakumana ndi ndende.Mtunda wapakati pa nsonga iyi ndi mphambano ya ma nkhwangwa ukuyimira kuchuluka kwa nickel mu Sample solution.
Njira zolandirira: NMT 1 ppm
• KUYATSA ZOSAVUTA <281>: NMT 0.1%, yotsimikizika pa gawo la 1.5g
KUCHEPETSA MASUKA
[Dziwani-Ndalama zomwe zatsimikizidwa pachiyesochi sizinaphatikizidwe mu ndalama zomwe zawerengedwa pansi pa Zonyansa Zina mu Zidziwitso Zazikulu.]
Yankho lachitsanzo: Sungunulani 3.3 g wa Sorbitol mu 3 ml ya madzi mothandizidwa ndi kutentha pang'ono.Kuziziritsa, ndikuwonjezera 20.0 mL ya cupric citrate TS ndi mikanda yagalasi yochepa.Kutenthetsa kuti kuwira kuyambike pambuyo pa 4 min, ndikupitirizabe kuwira kwa 3 min.Kuziziritsa mwachangu, ndipo onjezerani 40 mL wa acetic acid wosungunuka, 60 mL madzi, ndi 20.0 mL wa 0.05 N ayodini VS.Ndi kugwedeza kosalekeza, onjezerani 25 ml ya osakaniza 6 mL wa hydrochloric acid ndi 94 mL madzi.
Kuwunika: Madziwo akasungunuka, tsitsani ayodini wochulukirapo ndi 0,05 N sodium thiosulfate VS pogwiritsa ntchito 2mL wa wowuma TS, wowonjezedwa kumapeto kwa titration, ngati chizindikiro.
Njira zolandirira: NLT 12.8 mL ya 0.05 N sodium thiosulfate VS ndiyofunika, yolingana ndi NMT 0.3% ya kuchepetsa shuga, monga shuga.
• CHLORIDEAND SULFATE, Chloride<221> (ngati yalembedwa kuti igwiritsidwe ntchito pokonzekera mafomu a mlingo wa parenteral)
Chitsanzo: 1.5 g
Njira zolandirira: Chitsanzochi sichikuwonetsa chloride yochulukirapo kuposa 0.10 mL ya 0.020 N hydrochloric acid (NMT 0.0050%).
• CHLORIDEAND SULFATE, Sulfate <221> (ngati yalembedwa kuti igwiritsidwe ntchito pokonzekera mafomu a mlingo wa parenteral)
Chitsanzo: 1.0 g
Njira zolandirira: Chitsanzochi sichikuwonetsa sulfate yochulukirapo kuposa 0.10 mL ya 0.020 N sulfuric acid (NMT 0.01%).
MAYESO AKE
• MAYESERO A MICROBIAL ENUMERATION <61> ndi KUYESA KWA MIKROORGANISMS YOLAMBIDWA <62>: Chiwerengero chonse cha aerobic pogwiritsa ntchito Plate Method ndi NMT 1000 cfu/g, ndipo kuchuluka kwa nkhungu ndi yisiti zophatikiza ndi NMT 100 cfu/g
• PH <791>: 3.5-7.0, mu 10% (w/w) yankho m'madzi opanda carbon dioxide
• KUSINTHA KWA MADZI, Njira I <921>: NMT 1.5%
CLARITYAND COLOROF SOLUTION (ngati yalembedwa kuti igwiritsidwe ntchito pokonzekera mafomu a mlingo wa makolo)
Chitsanzo: 10.0 g
Kuwunika: Sungunulani Chitsanzocho mu 100.0 mL yamadzi opanda mpweya woipa.
Njira zovomerezera: Yankho lake ndi lomveka bwino komanso lopanda mtundu.
• KUYESA KWA MA BACTERIAL ENDOTOXINS <85> (ngati alembedwa kuti agwiritsidwe ntchito pokonzekera mafomu a mlingo wa makolo): NMT 4 USP Endotoxin Units/g ya mafomu a mlingo wa parenteral okhala ndi mulingo wosakwana 100g/L wa sorbitol, ndi NMT 2.5 USP Endotoxin Units/g kwa parenteral mlingo mitundu kukhala ndende ya 100g/L kapena kuposa sorbitol.
ZOWONJEZERA ZOFUNIKA
• PACKAGINGAND CHAGE: Sungani m’zotengera zotsekedwa bwino.Palibe zofunikira zosungira zomwe zafotokozedwa.
• KUYAMBIRA LEBO: Sorbitol yogwiritsidwa ntchito popanga mafomu a mlingo wa makolo ndi olembedwa.
MFUNDO ZA USP REFERENCE <11>
USP Endotoxin RS
USP Sorbitol RS