Berberine hydrochlorideyog xam nyob rau hauv qhuav qhuav, cov ntsiab lus ntawm C20H18ClNO4 nyob rau hauv lub extract yuav tsum tsis txhob tsawg tshaj li 97%.
【Properties】 Cov khoom no yog daj crystalline hmoov; odorless, iab heev.
Cov khoom no yaj hauv dej kub, me ntsis soluble hauv dej los yog ethanol, me ntsis soluble hauv chloroform, thiab insoluble hauv ether.
【Identification】 (1) Siv li ntawm 0.1g ntawm cov khoom no, ntxiv 10ml dej, maj mam cua sov kom yaj, ntxiv 4 tee ntawm sodium hydroxide tov, txias ( lim yog tsim nyog), ntxiv 8 tee ntawm acetone, thiab turbidity yuav tshwm sim.
(2) Siv li 5mg ntawm cov khoom no, ntxiv 2ml ntawm dilute hydrochloric acid, do, thiab ntxiv ib me me ntawm cov tshuaj bleaching, thiab nws yuav tig cherry liab.
(3) Noj li 2 mg ntawm cov khoom no, muab tso rau hauv ib lub tais dawb porcelain, ntxiv 1 ml ntawm sulfuric acid kom yaj nws, ntxiv 5 tee ntawm 5% gallic acid ethanol tov, rhaub nws nyob rau hauv ib da dej, thiab nws yuav. qhia emerald ntsuab.
(4) Lub teeb liab absorption spectrum ntawm cov khoom no yuav tsum ua raws li kev siv spectrum (spectral collection 320).
(5) Siv li ntawm 0.1 g ntawm cov khoom no, ntxiv 20 ml dej, maj mam sov kom yaj nws, ntxiv 0.5 ml ntawm nitric acid, txias nws, cia nws sawv ntsug rau 10 feeb. , lim nws, thiab cov filtrate yuav qhia txog cov tshuaj chloride (1) cov tshuaj tiv thaiv (Appendix III).
【Kev soj ntsuam】 Lwm cov alkaloids Siv cov khoom no, hnyav kom raug, yaj hauv ethanol thiab dilute los ua cov tshuaj uas muaj txog 2.0 mg rau 1 ml, raws li cov tshuaj ntsuam xyuas; noj jatrorrhizine siv tshuaj thiab bamipine siv tshuaj, ntsuas kom raug, yaj hauv ethanol thiab dilute los ua cov tshuaj uas muaj 0.10 mg thiab 0.04 mg ib 1 ml feem, raws li kev siv tshuaj. Raws li cov txheej txheem nyias txheej chromatography (Appendix Ⅴ B), noj 3ul ntawm cov tshuaj ntsuam xyuas thiab cov tshuaj jatrorrhizine siv, thiab pom lawv ntawm tib silica gel G nyias txheej phaj uas muaj 0.1% sodium carboxymethyl cellulose ua cov nplaum, thiab siv ethyl acetate. -chloroform-methanol-diethylamine (8: 2: 2: 1) ua tus neeg sawv cev tsim tawm. Tsim thiab tshuaj xyuas tam sim ntawd. Yog tias cov tshuaj ntsuam xyuas pom cov pob jatrorrhizine, lawv yuav tsum tsis txhob tsaus dua li cov xim ntawm cov chaw tseem ceeb ntawm kev siv tshuaj. Noj 3ul ntawm cov tshuaj ntsuam xyuas thiab cov tshuaj siv bamipine, raws li, thiab pom lawv ntawm tib lub silica gel G nyias txheej phaj uas muaj 0.1% sodium carboxymethyl cellulose ua cov nplaum, thiab siv n-butanol-glacial acetic acid-dej (7: 1: 2) raws li tus neeg sawv cev tsim, tsim, qhuav, thiab tshuaj xyuas nyob rau hauv lub teeb ultraviolet (365nm). Yog hais tias cov tshuaj ntsuam xyuas pom cov impurity me ntsis sib xws rau cov kev siv tshuaj, nws cov fluorescence siv yuav tsum tsis txhob muaj zog tshaj qhov chaw tseem ceeb ntawm cov ntaub ntawv siv tshuaj (cov khoom rho tawm).
Cyanide Noj 0.5g ntawm cov khoom no thiab xyuas nws raws li txoj cai (Tshooj Ntxiv VIII F Txoj Kev 1), uas yuav tsum ua kom tau raws li qhov yuav tsum tau ua (cov khoom siv hluavtaws).
Organic nitrile: Siv {{{0}}}.25g ntawm cov khoom hauv av finely, hnyav nws kom raug, muab tso rau hauv 25ml stoppered conical hwj, ntxiv 5ml ntawm anhydrous ether, co nws rau 5 feeb, lim nws nrog ib tug phoov. sintered funnel (G5), ntxuav nws nrog anhydrous ether 3 mus rau 4 zaug (2ml txhua lub sij hawm), muab cov filtrate thiab cov kua ntxhua, thiab mloog zoo rau txog li ntawm 0.5ml raws li cov tshuaj ntsuam xyuas; noj cov kua txob acetonitrile siv tus qauv tsim nyog, ntsuas nws kom raug, yaj nws hauv chloroform thiab dilute nws los ua cov tshuaj uas muaj txog 0.1mg ib 1ml, raws li kev siv tshuaj, raws li cov txheej txheem nyias nyias chromatography ( Cov ntawv ntxiv Ⅴ B), noj 10ul ntawm cov tshuaj siv thiab tag nrho cov nqi ntawm cov tshuaj ntsuam xyuas, raws li, pom lawv ntawm tib silica gel G (thickness 0.5mm) nyias txheej phaj, siv benzene-glacial acetic acid (25:0.1) raws li tus neeg sawv cev tsim, tsim nws, qhuav nws, thiab tshuaj tsuag nrog 5% ammonium molybdate sulfuric acid tov, rhuab ntawm 105 degree rau 10-20 feeb, tshuaj xyuas, cov tshuaj ntsuam xyuas yuav tsum tsis txhob qhia impurity me ntsis (cov khoom siv hluavtaws) ntawm qhov sib thooj ntawm cov chaw tseem ceeb uas qhia los ntawm kev siv tshuaj.
Poob ntawm ziab Siv cov khoom no thiab ziab nws ntawm 100 degree rau 5 teev, qhov hnyav poob yuav tsum tsis pub tshaj 12.0%.
Cov residue ntawm ignition Siv 1.0g ntawm cov khoom no thiab xyuas nws raws li txoj cai, cov seem seem yuav tsum tsis pub tshaj 0.2% (extract) los yog 0.1% ( cov khoom siv hluavtaws).
Hnyav hlau Siv cov khoom seem nyob rau hauv cov khoom seem ntawm qhov hluav taws kub thiab xyuas nws raws li txoj cai (Appendix Ⅷ H thib ob txoj kev), cov ntsiab lus ntawm cov hlau hnyav yuav tsum tsis pub tshaj 20 feem ntawm ib lab (cov khoom siv hluavtaws).
[Cov ntsiab lus txiav txim] Siv li ntawm {{{0}}.3g ntawm cov khoom no, ntsuas kom raug, muab tso rau hauv lub beaker, ntxiv 150ml ntawm boiling dej kom yaj, cia nws txias, Hloov nws mus rau 250ml volumetric hwj, kom raug ntxiv 50ml ntawm poov tshuaj dichromate titrant (0.016 67mol / L), dilute nws mus rau lub teev nrog dej, co nws rau 5 feeb, lim nws Nrog cov ntawv lim qhuav, ntsuas kom raug 100ml ntawm cov lim dej, muab tso rau hauv 250ml stoppered conical flask, ntxiv 2g ntawm poov tshuaj iodide, co nws kom dissolve nws, ntxiv 10ml ntawm hydrochloric acid tov (1 → 2), stopper nws nruj nreem, co. nws zoo, muab tso rau hauv qhov chaw tsaus rau 10 feeb, titrate nrog sodium thiosulfate titrant (0.1mol / L), ntxiv 2ml ntawm cov hmoov txhuv nplej siab thaum nws nyob ze rau qhov kawg taw tes, thiab txuas ntxiv mus rau titrate kom txog thaum cov xim xiav ploj. thiab qhov kev daws teeb meem tig ntsuab ntsuab, thiab kho qhov txiaj ntsig titration nrog kev sim dawb. Txhua 1ml ntawm potassium dichromate titration tov (0.016 67mol/L) yog sib npaug rau 12.39mg ntawm C20H18ClNO4.
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