I-Saccharin I-Insoluble CAS 81-07-2 Ubunyulu > 99.0% (HPLC)

Saccharin
C7H5NO3S 183.18
1,2-Benzisothiazol-3 (2H)-enye, 1,1-dioxide;
1,2-Benzisothiazolin-3-enye 1,1-dioxide [81-07-2].
INGCACISO
I-Saccharin iqulethe i-NLT 99.0% kunye ne-NMT 101.0% ye-C7H5NO3S, ibalwe ngokomisiweyo.
UKUCHAZA
• I-Infrared Absorption <197K>
UVAVANYO
• Inkqubo
Isampulu: 500 mg
Uhlalutyo: Susa iSampulu kwi-40 mL yotywala.Yongeza i-40 mL yamanzi kunye ne-phenolphthalein TS.Titrate nge-0.1 N sodium hydroxide.Yenza i-titration engenanto, ukuba kuyimfuneko, kwaye wenze ulungiso olufanelekileyo.I-mL nganye ye-0.1 N i-sodium hydroxide ilingana ne-18.32 mg ye-C7H5NO3S.
Indlela yokwamkela: 99.0% -101.0% kwisiseko esomileyo
UBUNGCOLA
Ukungcola Kwezinto Eziphilayo
• Intsalela kuKulayita <281>: NMT 0.2%.Ubushushu bomlilo bungama-600 ± 50.
• Iintsimbi ezinzima, Indlela II <231>: NMT 10 ppm
Ukungcola Okuphilayo
• Inkqubo 1: Umda weToluenesulfonamides
Isisombululo somgangatho wangaphakathi: 0.25 mg / mL ye-caffeine kwi-methylene chloride
Isisombululo sesitokhwe esisemgangathweni: 20.0 µg/mL ye-USP o-Toluenesulfonamide RS kunye ne-20.0 µg/mL ye-USP p-Toluenesulfonamide RS kwi-methylene chloride
Isisombululo esisemgangathweni: Phuma i-5.0 mL yesisombululo sesitokhwe esiPhakathi ukuze somele kumjelo wenitrogen.Nciphisa intsalela kwi-1 mL yesisombululo somgangatho wangaphakathi.
Isisombululo sesampuli: Nxiba i-10 g ye-Saccharin kwi-20 mL yamanzi, kwaye uchithe usebenzisa i-5-6 mL ye-10 N sodium hydroxide.Ukuba kuyimfuneko, lungisa isisombululo kunye ne-1 N sodium hydroxide okanye i-1 N hydrochloric acid kwi-pH ye-7-8, kwaye uhlambulule ngamanzi kwi-50 mL.Vuthulula isisombululo ngezixa ezine nganye ye-50 mL ye-methylene chloride.Hlanganisa iileyile ezisezantsi, zome phezu kwe-anhydrous sodium sulfate, kunye nesihluzo.Hlamba isihluzo kunye ne-sodium sulfate nge-10 mL ye-methylene chloride.Dibanisa isisombululo kunye nokuhlamba, kwaye umphunga uphantse wome kwindawo yokuhlambela amanzi kwiqondo lokushisa elingagqithiyo kuma-40. Ukusebenzisa inani elincinci le-methylene chloride, ngokobungakanani udlulisele intsalela kwityhubhu efanelekileyo ye-10-mL, iphuphuma ibe yomile kumlambo we initrogen, kwaye inyibilikise intsalela kwi-1.0 mL yesisombululo somgangatho waNgaphakathi.
Isinyibiliko esingenanto: Phuma i-200 mL ye-methylene chloride ukuze yome kwibhafu yamanzi kwiqondo lobushushu elingagqithiyo kuma-40. Nyibilikisa intsalela kwi-1 mL ye-methylene chloride.
Inkqubo yeChromatographic
(Jonga iChromatography <621>, Ukufaneleka kweNkqubo.)
Indlela: GC
Umtshina: Iionization yomlilo
Uluhlu: 0.53-mm × 10-m ikholamu yesilica edityanisiweyo, iqatywe ngesigaba se-G3 (ubukhulu befilimu 2 µm)
Ubushushu
Isitofu: 250
Umtshina: 250
Uluhlu: 180
Irhasi yokuthwala: Nitrogen
Izinga lokuhamba: 10 mL / min
Ubungakanani bokutofa: 1 µL
Umlinganiselo wokwahlula: 2:1
Ukufaneleka kwenkqubo
Iisampulu: Isisombululo esisemgangathweni kunye nesisombululo esingenanto
[Qaphela-Amachiza ahlanjululwa ngolu hlobo lulandelayo: o-toluenesulfonamide, p-toluenesulfonamide, kunye necaffeine.]
Iimfuno zokufaneleka: Akukho zincopho kumaxesha okugcina umgangatho wangaphakathi, i-o-toluenesulfonamide, okanye i-p-toluenesulfonamide;Isisombululo esingenanto
Isisombululo: NLT 1.5 phakathi kwe-o-toluenesulfonamide kunye ne-p-toluenesulfonamide, isisombululo esisemgangathweni
Uhlalutyo
Iisampulu: Isisombululo esisemgangathweni kunye nesisombululo seSampuli
Iinqobo zokwamkela: Ukuba naziphi na iincopho ngenxa ye-o-toluenesulfonamide kunye ne-p-toluenesulfonamide zivela kwichromatogram efunyenwe kunye nesisombululo seSampuli, umlinganiselo weendawo zabo kulowo wesisombululo somgangatho waNgaphakathi yi-NMT umlinganiselo ohambelanayo kwikhromatogram efunyenwe kunye nesisombululo esiPhakathi. .
Ukungcola komntu ngamnye: Jonga iTheyibhile yoku-1 yokungacoceki.
Itheyibhile yokungcola 1
Iinqobo zokwamkelwa kwegama (ppm)
o-Toluenesulfonamide 10
p-Toluenesulfonamide 10
• Inkqubo yesi-2: Umda weBenzoate kunye neSalicylate
Isisombululo sesampuli: 10 mL yesisombululo esishushu, esigcweleyo se-saccharin
Uhlalutyo: Yongeza i-ferric chloride TS dropwise kwisisombululo seSampule.
Indlela yokwamkela: Akukho mbala wemvula okanye i-violet ibonakala kulwelo.
IIMVAVANYO EZITHILE
• Uluhlu olunyibilikayo okanye iqondo lobushushu 741: 226-230
• Ilahleko ekomisweni <731>: Yomisa isampulu nge-105 nge-2 h: ilahlekelwa yi-NMT 1.0% yobunzima bayo.
• UVavanyo lweZinto eziKharboniza ngokulula 271
Isisombululo sesampuli: 40 mg / mL kwi-asidi ye-sulfuric (94.5% -95.5% [w / w] ye-H2SO4), igcinwe kwi-48-50 kwi-10 min
Iikhrayitheriya zokwamkelwa: Isisombululo seSampuli asinaso umbala ngaphezu koMatching Fluid A, xa sijongwa ngokuchasene nemvelaphi emhlophe.
• Ukucaca kwesisombululo
[Qaphela-Isicombululo seSampuli masithelekiswe noLungelelo lokunqunyanyiswa A kunye namanzi kwimini esasaziweyo emizuzwini emi-5 emva kolungiselelo lokunqunyanyiswa kweReferensi A.]
I-Diluent: i-200-g / L isisombululo se-acetate ye-sodium
Isisombululo se-Hydrazine: 10.0 mg / mL ye-hydrazine sulfate.[Qaphela-Vumela imele i4-6 h.]
Isisombululo seMethenamine: Dlulisa i-2.5 g ye-methenamine kwi-100-mL yeglasi-eyenziwe ngeglasi, yongeza i-25.0 mL yamanzi, faka isivalo seglasi, kwaye udibanise ukunyibilika.
Ukumiswa okuphambili kwe-opalescent: Dlulisa i-25.0 mL yesisombululo se-Hydrazine kwisisombululo se-Methenamine kwi-100-mL ye-glass-stoppered flask.Hlanganisa, kwaye uvumele ukuba ume i-24 h.[Qaphela-Olu kumiswa luzinzile kangangeenyanga ezi-2, ngaphandle kokuba lugcinwe kwisingxobo seglasi esingenaziphene.Ukumiswa akufanele kuhambelane neglasi kwaye kufuneka kuxutywe kakuhle ngaphambi kokusetyenziswa.Vumela ukunqunyanyiswa kume i-24 h.]
Umgangatho we-Opalescence: Nciphisa i-15.0 mL ye-Primary opalescent suspension ngamanzi ukuya kwi-1000 mL.[Qaphela-Oku kunqunyanyiswa akufuneki kusetyenziswe ngaphaya kweyure ezingama-24 emva kolungiselelo.]
Ukumiswa kwesalathiso A: Umgangatho we-Opalescence kunye namanzi (1 kuma-20)
Ukumiswa kwesalathiso B: umgangatho we-Opalescence kunye namanzi (1 kwi-10)
Isisombululo sesampuli: 200 mg / mL kwi-Diluent
Uhlalutyo
Iisampulu: Diluent, ukunqunyanyiswa kweReference A, ukunqunyanyiswa kweReferensi B, isisombululo sesampulu, kunye namanzi
Dlulisa inxalenye eyaneleyo yesisombululo seSampuli kwityhubhu yokuvavanya yeglasi engenambala, ecacileyo, engathathi hlangothi enesiseko esicaba kunye nobubanzi bangaphakathi be-15-25 mm ukufumana ubunzulu be-40 mm.Ngokukwanjalo tshintshela iinxalenye zeReferensi yokunqunyanyiswa A, ukunqunyanyiswa kweReferensi B, amanzi, kunye neDiluent ukwahlula iityhubhu zovavanyo oluhambelanayo.Thelekisa izisombululo ekukhanyeni kwemini esasazekileyo, ukujonga ngokuthe nkqo kwimvelaphi emnyama (jonga i-Spectrophotometry kunye ne-Light-Scattering 851, i-Visual Comparison).[Qaphela—Ukusasazwa kokukhanya kufuneka kube ngendlela yokuba ukunqunyanyiswa kweNgcombolo A kube lula ukwahlula emanzini, kwaye ukunqunyanyiswa kweNcwadana B kunokwahlulwa ngokulula kuNxibelelwano lokunqunyanyiswa A. ]
Indlela yolwamkelo: ISampuli yesisombululo sibonisa ukucaca okufanayo naleyo yamanzi, okanye i-Diluent, okanye i-opalescence yayo yi-NMT yoLungelelo lokunqunyanyiswa A.
• Umbala wesisombululo
I-Diluent A: isisombululo se-200-g / L se-acetate ye-sodium
I-Diluent B: isisombululo se-10-g / L se-hydrochloric acid
Isisombululo sesitokhwe esisemgangathweni: iFerric chloride CS, icobaltous chloride CS, cupric sulfate CS, kunye neDiluent B (3.0:3.0:2.4:1.6)
Isisombululo esisemgangathweni: Isisombululo esiqhelekileyo sesitokhwe kunye ne-Diluent B (1 kwi-100).[Qaphela-Lungisa isisombululo esiseMgangathweni ngokukhawuleza phambi kokusetyenziswa.]
Isisombululo sesampuli: Sebenzisa iSampuli isisombululo esivela kuvavanyo lokucaca kweSisombululo.
Uhlalutyo
Iisampulu: Diluent A, isisombululo esisemgangathweni, isisombululo sesampulu, kunye namanzi
Dlulisa inxalenye eyaneleyo yesisombululo seSampuli kwityhubhu yokuvavanya yeglasi engenambala, ecacileyo, engathathi hlangothi enesiseko esicaba kunye nobubanzi bangaphakathi be-15-25 mm ukufumana ubunzulu be-40 mm.Ngokufanayo ukudlulisa iinxalenye zesisombululo esiPhakathi, i-Diluent A, kunye namanzi ukuba ahlukane, adibanise iityhubhu zokuvavanya.Thelekisa izisombululo ekukhanyeni kwemini esasaziweyo, ukujonga ngokuthe nkqo kwimvelaphi emhlophe (jonga iSpectrophotometry kunye ne-Light-Scattering 851, Visual Comparison).
Iinqobo zokwamkela: Isisombululo seSampuli sinenkangeleko yamanzi okanye i-Diluent A, okanye ayinambala kakhulu kunesisombululo soMgangatho.
IIMFUNO EZONGEZELELWEYO
• Ukupakishwa kunye noGcino: Londoloza kwizikhongozeli ezivalwe kakuhle.Gcina kwiqondo lokushisa.
• IMigangatho yeReferensi ye-USP <11>
USP Saccharin RS Cofa ukujonga iSakhiwo
USP o-Toluenesulfonamide RS
USP p-Toluenesulfonamide RS