Cov luam yeeb muaj ntau yam alkaloids. Ntxiv rau cov ntsiab lus nicotine (muaj 2% ~ 8%), nws kuj muaj demethylnicotine (ie, nornicotine), anabasine (ie, anabasine) thiab tsawg kawg xya kab alkaloids. Nicotine yog lub hauv paus muaj nitrogen uas muaj ob hom heterocyclic, pyridine thiab pyrrole. Cov khoom lag luam ntshiab yog cov kua roj tsis muaj xim nrog lub qhov kub ntawm 246 degree, optically nquag (levorotatory), thiab soluble hauv dej thiab ntau cov kuab tshuaj organic.
Nicotine feem ntau muaj nyob rau hauv daim ntawv ntawm ntsev nrog cov organic acids xws li citric acid thiab malic acid nyob rau hauv cov nroj tsuag. Thaum muab rho tawm, luam yeeb feem ntau tuaj yeem ua kom sov nrog cov tshuaj inorganic muaj zog acid, thiab tom qab ntawd neutralized nrog alkali kom dawb nicotine. Tom qab ntawd rho tawm nrog cov kuab tshuaj organic, thiab evaporate cov kuab tshuaj kom tau nicotine. Vim nws yog volatile, nws tuaj yeem muab rho tawm los ntawm chav distillation.
Tsis tas li ntawd, vim nicotine yog kua, nws yog ib qho nyuaj rau cais thiab purify. Yog li ntawd, nicotine feem ntau hnov mob nrog picric acid los tsim nicotine dipicrate crystals rau kev ua haujlwm yooj yim.
I. Kev sim cov kauj ruam
(I) Steam distillation method
1. Cov khoom siv, tshuaj thiab cov khoom siv sim
(1) Cov cuab yeej 250mL puag ncig-hauv qab lub raj mis, 250mL beaker, 50mL conical flask, chav distillation apparatus, 200 degree ntsuas kub thiab ntsuas raj.
(2) Tshuaj thiab cov ntaub ntawv sim 5g qhuav luam yeeb hmoov av (los yog 5 luam yeeb yam tsis muaj ntawv), 10% tannic acid tov, 0.05% poov tshuaj permanganate tov, 10% sulfuric acid tov, iodine poov tshuaj iodide reagent, 30% sodium hydroxide tov, phenolphthalein, poov tshuaj mercuric iodide reagent, 20% acetic acid tov thiab saturated picric acid tov.
2. Kev rho tawm
Qhov hnyav 5g qhuav luam yeeb plua plav (los yog 5 luam yeeb yam tsis muaj ntawv) hauv 250mL beaker, ntxiv 50mL 10% sulfuric acid tov, do tsis tu ncua, thiab kub kom boil rau 20 feeb (Ceeb toom: ntxiv cov dej tsim nyog thaum boiling kom them nyiaj rau volatilization) . Tom qab txias me ntsis, maj mam ntxiv 30% sodium hydroxide tov (kwv yees li 40 mL) kom tshem tawm, thiab siv daim ntawv litmus los ntsuas kom txog thaum nws pom tseeb alkaline. Hloov cov sib tov rau hauv 250mL puag ncig-hauv qab khob thiab ntxiv 2 ~ 3 zeolites. Ua chav distillation. Nres distillation thaum txog 12 mL ntawm distillate tau sau. Ua cov cuab yeej sim ntawm lub distillate.
3. Cov khoom ntawm Nicotine
Siv rau lub raj kuaj huv huv, ntxiv 2 mL ntawm cov tshuaj nicotine rau txhua tus, thiab tom qab ntawd ua cov haujlwm hauv qab no:
(1) Ntxiv 1 poob ntawm phenolphthalein rau thawj lub raj kuaj. Kev hloov xim dab tsi tshwm sim?
(2) Ntxiv 1-2 tee ntawm 0.05% tshuaj poov tshuaj permanganate thiab 10 tee ntawm 10% sulfuric acid tov rau lub raj thib ob, co lub raj kuaj, thiab saib seb cov xim hloov li cas?
(3) Ntxiv 2 tee ntawm iodine potassium iodide reagent rau lub raj thib peb. Dab tsi tshwm sim tshwm sim?
(4) Ntxiv 5 tee ntawm saturated picric acid tov rau lub raj thib plaub. Dab tsi tshwm sim tshwm sim?
(5) Ntxiv 2-3 tee ntawm 10% tannic acid tov rau lub raj thib tsib. Dab tsi tshwm sim tshwm sim?
(6) Ntxiv 3 tee ntawm 20% acetic acid tov thiab 5 tee ntawm poov tshuaj mercuric iodide reagent rau lub thib rau lub raj. Dab tsi tshwm sim tshwm sim?
(II) Picrate Method
1. Cov khoom siv, tshuaj thiab cov khoom siv sim
(1) Cov cuab yeej lim dej, 150 mL cais funnel, 100 mL, 150 mL, 250 mL beakers, me ntxeem tau funnel, 50 mL conical hwj, iav ntaub plaub, lim ntawv, paj rwb ntaub plaub, dej da dej.
(2) Cov tshuaj thiab cov ntaub ntawv sim 8.5 g qhuav luam yeeb plua plav, 78 mL chloroform, methanol, saturated picric acid methanol tov, 5% sodium hydroxide tov.
2. Kev rho tawm
Ua kom raug hnyav 8.5 g qhuav luam yeeb plua plav thiab muab tso rau hauv 250 mL beaker, ntxiv 100 mL 5% sodium hydroxide tov, thiab do rau 20 feeb. Ncuav qhov sib tov rau hauv Buchner funnel (tsis muaj ntawv lim, tab sis nrog ib txheej ntawm iav ntaub plaub rau hauv qab) rau kev pom, thiab nyem cov pa luam yeeb plua plav kom nyem tawm ntau cov tshuaj alkali. Muab cov ntawv luam yeeb rov qab rau hauv lub khob qub, ntxiv 2 mL dej distilled (stirring) los ntxuav, thiab tom qab ntawd lim dua, thiab muab ob lub lim dej sib tov.
Hloov cov lim mus rau qhov sib cais thiab ntxiv 25 mL chloroform rau kev rho tawm. Maj mam co cov ntsiab lus ntawm qhov sib cais funnel, cia nws sawv ntsug thiab cais cov khaubncaws sab nraud povtseg. Muab cov txheej qis (theem organic) rau hauv 150mL beaker, thiab tshem tawm cov txheej sab saud (aqueous theem) ob zaug nrog 50mL chloroform. Muab peb cov extracts thiab ua tib zoo ncuav tag nrho cov extracts rau hauv 150mL puag ncig-hauv qab khob. Thaum tshav kub kub thiab distilled nyob rau hauv ib da dej da dej kom rov qab tau cov chloroform. Thaum 8 ~ 10mL ntawm cov tshuaj tso tseg, tam sim ntawd txias lub hwj thiab hloov tag nrho cov extracts mus rau 50mL puag ncig-hauv qab khob. Ntxuav thawj lub hwj nrog 3mL chloroform thiab muab tso rau hauv 50mL hwj. Thaum tshav kub kub thiab distilled nyob rau hauv ib da dej da dej kom mloog zoo rau dryness. Ib qho me me ntawm cov roj los yog cov khoom seem tshuav. Ntxiv 1mL ntawm cov dej distilled thiab co maj mam yaj cov residue. Ntxiv 4mL ntawm methanol (daj precipitate tam sim ntawd ua). Dhau cov tshuaj methanol no los ntawm lub funnel padded nrog iav ntaub plaub thiab lim nws mus rau hauv 100mL beaker, thiab ntxuav nws ib zaug nrog 5mL ntawm methanol (cov lim yuav tsum ntshiab tsis muaj teeb meem nyob rau lub sij hawm no, txwv tsis pub nws yuav tsum tau lim dua). Ntxiv 10 mL ntawm saturated picric acid methanol tov, thiab tam sim ntawd precipitate ib fluffy yellowish nicotine dipicrate. Lim nyob rau hauv lub siab txo siv lub me me ntxeem tau funnel los yog iav ntsia thawv funnel padded nrog lim ntawv.
Qhov hnyav: txog 50 mg.
3. Recrystalization
Muab cov tau txais nicotine dipicrate rau hauv 50 mL conical flask, thiab maj mam ntxiv kub 50% (ntim piv) ethanol-dej tov nyob rau hauv cua kub kom txog thaum cov khoom tsuas yog yaj. Cia sawv ntsug thiab txias, thiab ntev, ci daj prismatic crystals yuav tshwm sim (vim tias cov txheej txheem crystallization qeeb, nws yog qhov zoo tshaj rau ntsaws lub khob ntim nrog lub stopper thiab cia nws sawv ntsug kom txog rau thaum qhov kev sim tom ntej). Lim nyob rau hauv lub siab txo siv lub me me ntxeem tau funnel los yog iav ntsia thawv funnel padded nrog lim ntawv, thiab qhuav thaum hmo ntuj. Sau cov khoom thiab txiav txim siab lub melting point.