1, ho khetholla mokhoa oa hydroxypropyl methyl cellulose
(1) Nka 1.0g ea sampole, metsi a futhumetseng (80 ~ 90 ℃) 100mL, tsosa ka ho tsoelang pele, 'me u pholile ho ba mokelikeli oa viscous ka bateng ea leqhoa; Kenya 2mL ea mokelikeli ka har'a tube ea teko, butle-butle eketsa 1mL sulfuric acid solution ea 0.035% athrone haufi le lebota la tube, 'me u tsamaee bakeng sa 5min. Reng e tala e hlaha sehokelong pakeng tsa maro a mabeli.
(2) Nka palo e loketseng ea slime e boletsoeng ka holimo e sebelisitsoeng ho khetholla (ⅰ) 'me u e tšele holim'a poleiti ea khalase. Ka mor'a hore metsi a fetohe mouoane, filimi ea ductile e thehoa.
2, tlhahlobo ea hydroxypropyl methyl cellulose ea tokiso e tloaelehileng ea tharollo
(1) Sodium thiosulfate tharollo e tloaelehileng (0.1mol/L, bonnete: khoeli e le 'ngoe)
Boitokisetso: Pheha ka 1500mL metsi a silafetseng 'me u pholile ho fihlela u se u loketse ho sebelisoa. Beha boima ba 25g sodium thiosulfate (boima ba molek'hule ke 248.17, 'me u leke ho nepahala ho isa ho 24.817g ha u le boima) kapa 16g anhydrous sodium thiosulfate, e qhibilihe ka 200mL ea metsi a pholileng a ka holimo, e hlapolle ho 1L, 'me ue behe sebakeng se sootho. botlolo, beha botlolo lefifing, 'me e sefa hore e sebelisoe ka mor'a libeke tse peli.
Tekanyo: Boima ba 0.15g ea potassium dichromate e phehiloeng ka boima bo sa feleng, e nepahetseng ho isa ho 0.0002g. Kenya 2g potassium iodide le 20mL sulfuric acid (1+9), sisinya hantle, beha lefifing bakeng sa 10min, eketsa metsi a 150mL le 3ml 0.5% ea tharollo ea starch ea 0.5%, titrate ka 0.1mol / L sodium thiosulfate tharollo, tharollo e fetoha e putsoa. ho botala bo kganyang qetellong. Potassium chromate ha ea eketsoa tekong e se nang letho. Ts'ebetso ea ho lekanya e phetoa makhetlo a 2 ~ 3 mme boleng bo tloaelehileng bo nkiloe.
Molar concentration C (mol/L) ea sodium thiosulfate standard solution e baloa ka tsela e latelang:
Moo, M ke boima ba potassium dichromate; V1 ke molumo oa sodium thiosulfate e jeoang, mL; V2 ke bophahamo ba sodium thiosulfate e jetsoeng tekong e se nang letho, mL; 49.03 ke boima ba potassium dichromate bo lekanang le 1mol ea sodium thiosulfate, g.
Kamora ho lekanya, eketsa Na2CO3 e nyane ho thibela ho bola ha likokoana-hloko.
(2) Tharollo e tloaelehileng ea NaOH (0.1mol/L, ho sebetsa: khoeli e le 'ngoe)
Boitokisetso: Hoo e ka bang 4.0g ea NaOH e hloekileng bakeng sa tlhahlobo e ne e lekanngoa ka beaker, 'me metsi a 100mL a qhibilihisitsoeng a ile a kenngoa ho qhibiliha, ebe a fetisetsoa ho 1L volumetric flask,' me metsi a hloekisitsoeng a kenngoa sekaleng, 'me a behoa matsatsi a 7-10 ho fihlela. teka-tekano.
Calibration: Kenya 0.6 ~ 0.8g ea pure potassium hydrogen phthalate e omisitsoeng ho 120 ℃ (e nepahetseng ho 0.0001g) ka har'a 250mL conical flask, eketsa 75mL metsi a qhibilihisitsoeng ho e qhaqha, ebe u eketsa marotholi a 2 ~ 3 a 1% phenolphthalein. tharollo e ka holimo e lokiselitsoeng ea sodium hydroxide ho fihlela e le khubelu hanyenyane, 'me ntlha ea ho qetela ke hore' mala ha o felle ka har'a 30S. Ngola molumo oa sodium hydroxide. Ts'ebetso ea ho lekanya e phetoa ka makhetlo a 2 ~ 3 mme boleng bo tloaelehileng bo nkiloe. 'Me u etse teko e se nang letho.
Motsoako oa tharollo ea sodium hydroxide e baloa ka tsela e latelang:
Moo, C ke motsoako oa sodium hydroxide solution, mol/L; M e emetse boima ba potassium hydrogen phthalate, G; V1 ke molumo oa sodium hydroxide e jeoang, mL; V2 e emela boholo ba sodium hydroxide e sebelisoang tekong e se nang letho, mL; 204.2 ke boima ba molar ba potasiamo hydrogen phthalate, g ka mole.
(3) Hlakola sulfuric acid (1+9) (Ho sebetsa: khoeli e le 'ngoe)
Ha u ntse u hlohlelletsa, ka hloko eketsa 100mL concentrated sulfuric acid ho 900mL metsi a qhibilihisitsoeng, u eketsa butle, ha u ntse u hlohlelletsa.
(4) Hlakola sulfuric acid (1+16.5) (Ho sebetsa: likhoeli tse 2)
Ha u ntse u hlohlelletsa, eketsa ka hloko 100mL ea concentrated sulfuric acid ho 1650mL ea metsi a hloekisitsoeng, u eketsa butle. Hlohlelletsa ha u ntse u tsamaea.
(5) Letšoao la starch (1%, bonnete: matsatsi a 30)
Beha 1.0g starch e qhibilihang, eketsa 10mL ea metsi, hlohlelletsa le ho e kenya ka har'a 100mL ea metsi a belang, pheha hanyenyane bakeng sa 2mins, e behe, 'me u sebelise supernatant bakeng sa tšebeliso.
(6) Letšoao la starch
Pontšo ea 0.5% ea starch e fumanoe ka ho nka 5mL ea tharollo ea 1% ea starch e lokisitsoeng le ho e hlapolla ho 10mL ka metsi.
(7) 30% tharollo ea chromium trioxide (e sebetsang: khoeli e le 'ngoe)
Beha boima ba 60g ea chromium trioxide 'me u e qhale ka 140mL ea metsi ntle le lintho tse phelang.
(8) Tharollo ea Potassium acetate (100g/L, bonnete: Likhoeli tse 2)
10g ea lijo-thollo tsa anhydrous potassium acetate e ile ea qhaloa ka 100mL tharollo ea 90mL glacial acetic acid le 10mL acetic anhydride.
(9) 25% tharollo ea sodium ea acetate (220g/L, ho nepahala: likhoeli tse 2)
Qhala 220g ea anhydrous sodium acetate ka metsing 'me u hlapolle ho 1000mL.
(10) Hydrochloric acid (1:1, bonnete: likhoeli tse 2)
Kopanya concentrated hydrochloric acid le metsi ka karolelano ea 1: 1.
(11) Tharollo ea acetate buffer (pH=3.5, bonnete: likhoeli tse 2)
Qhala 60mL acetic acid ka metsing a 500mL, ebe o eketsa 100mL ammonium hydroxide mme o hlapolle ho 1000mL.
(12) Tharollo ea ho lokisetsa nitrate pele
159.8mg ea nitrate ea lead e ile ea qhibiliha ka metsing a 100mL a nang le 1mL ea nitric acid (density 1.42g / cm3), e hloekisitsoeng ho 1000mL ea metsi le e tsoakiloeng hantle. Ho lokisetsa le ho boloka tharollo ena ho tla etsoa ka khalase e se nang loto.
(13) Tharollo e tloaelehileng ea ho etella pele (ho sebetsa: likhoeli tse 2)
Tekanyo e nepahetseng ea 10mL ea tharollo ea loto ea nitrate e ile ea hlapolloa ka metsi ho ea ho 100mL.
(14) 2% tharollo ea hydroxylamine hydrochloride (nako ea ho sebetsa: khoeli e le 'ngoe)
Qhala 2g ea hydroxylamine hydrochloride ka 98mL ea metsi.
(15) Ammonia (5mol/L, ho sebetsa: likhoeli tse 2)
175.25g ea ammonia e ile ea qhibiliha ka metsing 'me ea hlapolloa ho 1000mL.
(16) Mokelikeli o tsoakiloeng (nako ea ho sebetsa: likhoeli tse 2)
Kopanya 100mL glycerol, 75mLNaOH tharollo (1mol/L), le 25mL metsi.
(17) Tharollo ea Thioacetamide (4%, bonnete: likhoeli tse 2)
4g thioacetamide e ile ea qhibiliha ka metsing a 96g.
(18) Phenanthroline (0.1%, bonnete: khoeli e le 'ngoe)
Hlakola 0.1g o-phenanthroline ka metsing a 100mL.
(19) Acid stannous chloride (ho sebetsa: khoeli e le 'ngoe)
Qhala 20g stannous chloride ka 50mL concentrated hydrochloric acid.
(20) Potassium hydrogen phthalate standard buffer solution (pH 4.0, bonnete: likhoeli tse 2)
10.12g ea potassium hydrogen phthalate (KHC8H4O4) e ne e lekantsoe hantle le ho omisoa ho (115±5) ℃ bakeng sa 2 ~ 3h. Hlatsoa ho 1000mL ka metsi.
(21) Tharollo e tloaelehileng ea phosphate buffer (pH 6.8, ho sebetsa: likhoeli tse 2)
3.533g ea anhydrous disodium hydrogen phosphate le 3.387g ea potassium dihydrogen phosphate e omisitsoeng ho (115±5) ℃ bakeng sa 2 ~ 3h li ile tsa lekanngoa hantle le ho hlapolloa ho 1000mL ka metsi.
3, boikemisetso ba litaba tsa sehlopha sa hydroxypropyl methyl cellulose
(1) Boikemisetso ba litaba tsa methoxy
Boikemisetso ba dikahare tsa methoxy bo ipapisitse le ho bola ha hydroiodate acid ka ho futhumatsa ka teko e nang le methoxy ho hlahisa iodide ea methane e sa fetoheng (ntlha e belang 42.5 ° C). Methane iodide e tšeloa ka naetrojene ka tharollo ea autoreaction. Ka mor'a ho hlatsoa ho tlosa lintho tse sitisang (HI, I2 le H2S), mouoane oa iodine oa methane o kenngoa ke potassium acetate acetic acid e nang le Br2 ho etsa IBr ebe o oxidized ho iodic acid. Ka mor'a hore ho be le distillation, lintho tse amohelehang li fetisetsoa libotlolong tsa iodine 'me li hlapolotsoe ka metsi. Ka mor'a ho eketsa formic acid ho tlosa Br2 e feteletseng, KI le H2SO4 li kenngoa. Likahare tsa methoxy li ka baloa ka ho etsa titrating 12 ka tharollo ea Na2S2O3. The reaction equation e ka hlalosoa ka tsela e latelang.
Sesebelisoa sa ho metha litaba tsa methoxy se bonts'itsoe ho Setšoantšo sa 7-6.
Ho 7-6 (a), A ke botlolo ea 50mL e chitja e tlase e hokahaneng le catheter. The bottleneck e hlomelloa ka ho otloloha ka moea o otlolohileng condensing tube tube E, e ka bang 25cm ka bolelele le 9mm ka hare bophara. Karolo e ka holimo ea tube e kobetsoe ka har'a tube ea capillary ea khalase e nang le sekoti se theohelang le bophara ba 2mm ka hare. Setšoantšo sa 7-6 (b) se bontša sesebelisoa se ntlafalitsoeng. 1 ke flask ea reaction, e leng 50mL e chitja e tlase, 'me peipi ea naetrojene e ka ho le letšehali. 2 ke phala e otlolohileng ea condensing; 3 ke scrubber, e nang le mokelikeli oa ho hlatsoa; 4 ke tube ea ho monya. Phapang e kholo ka ho fetisisa pakeng tsa sesebelisoa le mokhoa oa pharmacopoeia ke hore li-absorber tse peli tsa mokhoa oa pharmacopoeia li kopantsoe ho ba le le leng, tse ka fokotsang tahlehelo ea tharollo ea ho qetela ea ho monya. Ho phaella moo, mokelikeli oa ho hlatsoa ka scrubber o boetse o fapane le mokhoa oa pharmacopoeia, e leng metsi a hloekisitsoeng, 'me sesebelisoa se ntlafetseng ke motsoako oa cadmium sulfate solution le sodium thiosulfate solution, e ka khonang ho senya litšila tsa khase e silafetseng habonolo.
Pipette ea lisebelisoa: 5mL (5), 10mL (1); Borette: 50mL; Botlolo ea ho lekanya iodine: 250mL; Sekaseka ho leka-lekana.
Reagent phenol (hobane e tiile, kahoo e tla kopanngoa pele e fepa); naetrojene kapa carbon dioxide; Hydroiodate acid (45%); Analysis ea hloekileng; Tharollo ea potassium acetate (100g/L); Bromine: ho hloeka ha tlhahlobo; Formic acid: e hloekile ka ho hlahloba; 25% ea tharollo ea sodium ea acetate (220g / L); KI: bohloeki ba ho hlahloba; Hlakola sulfuric acid (1+9); Sodium thiosulfate tharollo e tloaelehileng (0.1mol/L); Phenolphthalein pontshi; 1% tharollo ea ethanol; Letšoao la starch: 0.5% starch metsing; Hlakola sulfuric acid (1 + 16.5); 30% tharollo ea chromium trioxide; Metsi a se nang lintho tse phelang: eketsa 10mL hlapolla sulfuric acid (1+16.5) ho 100mL ea metsi, mocheso ho bela, 'me u kenye 0.1ml0.02mol /L potassium permanganate titer, pheha bakeng sa 10min, e tlameha ho boloka pinki; 0.02mol/L sodium hydroxide titration solution: Ho latela mokhoa oa Sehlomathiso sa Pharmacopoeia oa China, 0.1mol/L sodium hydroxide titration solution e ile ea lekanngoa le ho hlapolloa ka nepo ho 0.02mol/L ka metsi a phehiloeng le a pholileng.
Eketsa hoo e ka bang 10mL ea tharollo ea ho hlatsoa ka har'a tube ea ho hlatsoa, eketsa 31mL ea tharollo e sa tsoa lokisoa ka har'a tube ea ho monya, kenya sesebelisoa, boima ba 0.05g (e nepahetseng ho isa ho 0.0001g) ea sampole e omisitsoeng e omisitsoeng ho boima bo sa feleng ho 105. ℃ ka har'a botlolo ea karabelo, 'me u kenye 5mL hydroiodate. Botlolo ea karabelo e hokahanngoa ka potlako ho condenser ea ho hlaphoheloa (molomo o silang o kolobisitsoe ka hydroiodate), 'me naetrojene e pompeloa ka tanka ka sekhahla sa li-bubble tse 1 ~ 2 motsotsoana. Mocheso o laoloa butle-butle e le hore mouoane oa mokelikeli o belang o nyolohele ho halofo ea bophahamo ba condenser. Nako ea karabelo e ipapisitse le mofuta oa sampole, lipakeng tsa 45min le 3h. Tlosa tšupu e monyang 'me u fetise ka hloko tharollo e monyang ka har'a botlolo ea iodine ea 500mL e nang le 10ml ea 25% ea sodium acetate solution ho fihlela kakaretso ea molumo e fihla hoo e ka bang 125mL.
Tlas'a ho sisinyeha kamehla, butle-butle eketsa lerotholi la acid ea formic ka lerotholi ho fihlela mosehla o nyamela. Kenya lerotholi la 0.1% methyl red indicator, 'me' mala o mofubelu ha o nyamele metsotso e 5. Ebe u eketsa marotholi a mararo a formic acid. E tlohele e lule nakoana, ebe u eketsa 1g ea potassium iodide le 5mL ea dilute sulfuric acid (1+9). Tharollo e ne e le titrated ka 0.1mol / L sodium thiosulfate tharollo e tloaelehileng, 'me marotholi a 3 ~ 4 a 0.5% ea starch indicator a eketsoa haufi le ntlha ea ho qetela,' me titration e ile ea tsoela pele ho fihlela 'mala o moputsoa o nyamela.
Boemong bo tšoanang, ho ile ha etsoa teko e se nang letho.
Palo ea kakaretso ea methoxide content:
Moo, V1 e emelang bophahamo ba modumo (mL) ya sodium thiosulfate standard solution e jewang ke disampole tsa titration; V2 ke boholo ba tharollo e tloaelehileng ea sodium thiosulfate e sebelisoang litekong tse se nang letho, mL; C ke motsoako oa sodium thiosulfate standard solution, mol/L; M e bua ka boima ba sampole e omisitsoeng, g; 0.00517 ke 0.1mol / L sodium thiosulfate ka 1ml e lekanang le 0.00517g ea methoxy.
Kakaretso ea methoxy e emela kakaretso ea methoxy le boleng ba hydroxyproxy ea lipalo tsa methoxy, kahoo alkoxy eohle e tlameha ho lokisoa ke sephetho sa hydroxyproxy content ho fumana methoxy e nepahetseng. LITENG HAHYDROXYPROPOXY E LOKELA HO LOKELANG HO HLOKAHALA HO PROPENE E HLAHISITSANG KE KATSO EA HI LE HYDROXYPROPYL LE CONSTANT K=0.93 (MOHOO OA LINTHO TSE KHOLO EA lisampole tse KHETHANG KE MOKHOA OA Morgan). Ka hona:
Likahare tsa methoxy tse lokisitsoeng = kakaretso ea methoxy - (litaba tsa hydroxypropoxy × 0.93×31/75)
Moo palo ea 31 le 75 e leng bongata ba molar ea lihlopha tsa methoxy le hydroxypropoxy, ka ho latellana.
(2) Boikemisetso ba litaba tsa hydroxypropoxy
Sehlopha sa hydropropoxy sampoleng se kopana le chromium trioxide ho hlahisa asiti ea acetic. Kamora ho hloekisoa ho tsoa tharollong ea autoreaction, litaba tsa chromic acid li khethoa ke titration ka tharollo ea NaOH. Hobane karolo e nyane ea chromic acid e tla hlahisoa ts'ebetsong ea distillation, tharollo ea NaOH e tla boela e jeoe, kahoo litaba tsa chromic acid ena li lokela ho khethoa ka ho eketsehileng ke iodimetry le ho tlosoa ho palo. Reaction equation ke:
Lisebelisoa le li-reagents Sehlopha se feletseng sa lisebelisoa bakeng sa boikemisetso ba lihlopha tsa hydroxypropoxy; Botlolo ea volumetric: 1L, 500mL; Moqomo oa ho lekanya: 50mL; Pipette: 10mL; Botlolo ea ho lekanya iodine: 250mL. Freette ea motheo: 10mL; Sodium thiosulfate tharollo e tloaelehileng (0.1mol/L); Hlakola sulfuric acid (1 + 16.5); Hlakola sulfuric acid (1+9); Letšoao la starch (0.5%).
7-7 ke sesebelisoa sa ho tseba litaba tsa hydroxypropoxy.
Ho 7-7 (a), D ke botlolo ea 25mL e nang le melala e habeli, B ke 25mm×150mm jenereithara ea mouoane, C ke phallo ea khokahanyo, A ke bate ea oli e futhumatsang ea motlakase, E ke kholomo ea shunt, G ke botlolo ea conical e nang le plug ea khalase, bophara bo ka hare bo qetellang ke 0.25-1.25mm, e kenngoa ka har'a botlolo ea distilling; F ke tšupu e kopanyang e hoketsoeng ho E. Ka sesebelisoa se ntlafalitsoeng se bontšitsoeng ho FIG. 7-7 (b), 1 ke setsi sa motlakase, e leng 50mL distillation flask; 2 ke hlooho ea distillation; 3 ke mochini oa khalase oa 50mL ho laola lebelo la phallo ea metsi a tlhaho; 4 ke phala ea naetrojene; 5 ke phala e kokobetsang. Phapang ea bohlokoa ka ho fetisisa pakeng tsa sesebelisoa se fetotsoeng le mokhoa oa pharmacopoeia ke ho eketsoa ha lesela la khalase ho laola lebelo la ho phalla ha metsi, e le hore tekanyo ea distillation e ka laoloa habonolo.
Mekhoa ea liteko ea sampole ea 105 ℃ ho omisa ho boima bo sa feleng e ka ba 0.1 g (0.0002 g), e nepahetseng e boletse ka botlolong ea distillation, eketsa 10 ml ea 30% chromium trioxide solution, botlolo ea distillation ka senoelong sa bate ea oli, boemo ba mokelikeli oa ho hlapa oli. e lumellanang le chromium trioxide liquid surface, lisebelisoa tse kentsoeng, metsi a pholileng a bulehileng, naetrojene, ea fektheri ea rona ho laola sekhahla sa nitrogen hoo e ka bang bubble e le 'ngoe ka motsotsoana. Nakong ea 30min, bate ea oli e ne e futhumatsoa ho 155 ℃ 'me e bolokoe mocheso ona ho fihlela tharollo e bokelitsoeng e fihla ho 50mL. The distillation e ile ea emisoa ho tlosa bate ea oli.
Hlatsoa lebota le ka hare la pholileng ka metsi a hloekisitsoeng, kopanya metsi a hlatsoang le distillate ka botlolo ea iodine ea 500mL, eketsa marotholi a 2 a 1% phenolphthalide indicator, titrate le 0.02mol / L sodium hydroxide solution ho pH bohlokoa ba 6.9 ~ 7.1 , 'me u ngole palo eohle ea sodium hydroxide e sebelisitsoeng.
Kenya 0.5g sodium bicarbonate le 10mL hlapolla sulfuric acid (1+16.5) botlolong ea iodine 'me e eme ho fihlela ho se na carbon dioxide e hlahisoang. Ebe u eketsa 1.0g iodide ea potasiamo, ue kopanye ka thata, e sisinye hantle 'me ue tlohele lefifing bakeng sa 5min. Ebe u eketsa 1mL 0.5% letšoao la starch 'me u le titrate ka 0.02mol / L sodium thiosulfate ho fihlela qetellong. Ngola palo ea sodium thiosulfate e sebelisitsoeng.
Tekong e 'ngoe e se nang letho, linomoro tsa sodium hydroxide le sodium thiosulfate titrators tse jetsoeng li tlalehiloe ka ho latellana.
Palo ea litaba tsa hydroxypropoxy:
Moo, K e leng setšoantšo sa coefficient sa tokiso sa teko e se nang letho: V1 ke molumo oa sodium hydroxide titration e sebelisoang ke sampole, mL. C1 ke motsoako oa sodium hydroxide standard solution, mol/L; V2 ke molumo oa sodium thiosulfate titration e sebelisoang ke sampole, mL; C2 ke motsoako oa sodium thiosulfate standard solution, mol/L; M ke sampole boima, g; Va ke molumo oa sodium hydroxide titration e sebelisoang litekong tse se nang letho, mL; Vb ke molumo oa sodium thiosulfate titration e sebelisitsoeng tekong e se nang letho, mL.
4. Boikemisetso ba mongobo
Tekanyo ea tlhahlobo ea lisebelisoa (e nepahetseng ho 0.1mg); Botlolo ea ho lekanya: bophara ba 60mm, bolelele ba 30mm; Ho omisa onto.
Mokhoa oa teko o lekanya ka nepo sampole 2~ 4G (
Nako ea poso: Sep-08-2022