Kev Txhim Kho Ntawm Tag Nrho Flavonoids Los Ntawm Cistanche Deserticola Los Ntawm MOF Cov Khoom

Abstract Cistanche deserticola YC Ma, raws li ib txwm "zaub mov thiab tshuaj" tshuaj ntsuab tshuaj ntsuab, yog yus muaj los ntawm nws cov flavonoids, uas muaj immunomodulatory thiab antioxidant teebmeem. Hauv txoj kev tshawb no, peb tau tshawb xyuas qhov kev ua tau zoo ntawm MOFs sib txawv hauv kev txhim kho thiab sib cais ntawm tag nrho cov flavonoids los ntawmCistanche deserticola Y.C. Ma thiab qhov zoo tshaj plaws adsorptionand daws teeb meem. Tsib MOFs, [Zn(nicotinate)2]n, MIL-101(Cr), MIL-101(Fe), MIL-53(Fe) thiab MOF-5, tau ua ke los ntawm hydrothermal synthesis, thiab tus cwj pwm los ntawm PXRD, FT-IR, SEM thiab TG los xyuas kom meej cov synthesis yog, thiab cov adsorption thiab desorption ntau npaum li cas nyob rau hauv txawv tej yam kev mob raug coj raws li lub Performance index rau ntsuam xyuas adsorption thiab desorption kev ua tau zoo. Tom qab kev tshuaj ntsuam xyuas, zinc nicotinate coordination polymer [Zn(nicotinate) 2]n ([Zn(NA)2]) tau pom tias muaj kev ua tau zoo tag nrho thiab kev pom zoo adsorption thiab desorption tej yam kev mob raug txiav txim. Cov txiaj ntsig tau pom tias qhov zoo tshaj plaws adsorption tej yam kev mob yog adsorption lub sij hawm ntawm 6 h, pH tus nqi ntawm cov qauv Tshuag tov ntawm 5. tag nrhoFlavonoids ntawm Cistanchis sinensislos ntawm [Zn(NA)2] yog 62.91 mg∙mL-1. Qhov zoo tshaj plaws desorption mob yog 30% ethanol tov, thiab tus nqi desorption yog 45.52%. Lub purity ntawm tag nrho cov flavonoids nyob rau hauv Cistanche tau nce los ntawm 9.33% mus rau 48.23% tom qab adsorption thiab desorption. Thecrystalline daim ntawv ntawm [Zn(NA)2] ua ntej thiab tom qab adsorption thiab desorption yog tus cwj pwm los ntawm PXRD li ruaj khov. Cov kev sim tau pom tias [Zn(NA)2] tau nthuav tawm cov kev ua haujlwm siab adsorption nrog kev ua kom muaj txiaj ntsig zoo thiab ua kom huv ntawm cov flavonoids los ntawm Cistanche. Yog li ntawd, MOFs muaj ntau yam ntawm daim ntawv thov kev cia siab raws li cov ntaub ntawv tawm tshiab rau kev txhim kho thiab kev sib cais ntawm cov khoom xyaw nquag hauv cov tshuaj suav tshuaj.

Ntsiab lus:Hlau Organic Frameworks (MOFs);Cistanche deserticola;tag nrho cov flavonoids

HERBAL CISTANCHE nrog HIGH-QibFlavonoids

Cistanche deserticola YC Ma[1] yog ib tsob nroj uas muaj npe nyob rau hauv "khoom noj thiab tshuaj homology" catalog ntawm National Health Commission[2]. Nws yog lub npe hu ua "desert ginseng"[3] thiab muaj ntau yam haujlwm, xws litxhim khu kev tiv thaivthiabneurotiv thaiv[4-9]. Nws cov khoom xyaw tseem ceeb yog flavonoids, uas muaj ntau yam haujlwm lom neeg xws lianti-inflammatory thiab tiv thaiv kab mob kev cai[10-13]. Txoj kev sib cais ib txwm muaj ntau yam tsis zoo, xws li kev ua haujlwm nyuaj thiab kev siv hnyav[14-17]. Hlau organic moj khaum (MOFs) cov ntaub ntawv tau txais kev kawm dav vim lawv qhov loj me ntawm thaj chaw tshwj xeeb thiab muaj peev xwm adsorption muaj zog, qhia lawv lub peev xwm ntawm adsorption thiab kev sib cais ntawm cov tshuaj suav tshuaj [18-26]. Hauv txoj kev tshawb no, zinc nicotinate coordination polymer ([Zn(NA)2]) raug xaiv los ua tus adsorbent los tshawb txog nws cov nyhuv adsorption ntawm tag nrho cov flavonoids los ntawm Cistanche deserticola thiab kev pom zoo adsorption thiab tsom xam cov xwm txheej. Lub hom phiaj yog los muab kev txhawb nqa theoretical rau kev sib cais thiab kev nplua nuj ntawm tag nrho cov flavonoids los ntawm Cistanche deserticola, nthuav cov ntawv thov ntawm MOFs cov ntaub ntawv hauv kev txhim kho thiab kev sib cais ntawm cov tshuaj suav tshuaj, thiab tsim kom muaj kev lag luam, ib puag ncig zoo thiab muaj txiaj ntsig sib cais thiab purification txoj kev.

1 Kev sim ib feem

1.1 Instruments thiab reagents

Cistanche deserticola, yuav los ntawm Beijing Tongrentang Pharmacy; rutin, tus qauv tshuaj, yuav los ntawm Tuam Tshoj Food and Drug Administration; niacin, analytical qib, yuav los ntawm Tianjin Bodi Chemical Co., Ltd.; sodium hydroxide; anhydrous ethanol; sodium nitrite; zinc sulfate heptahydrate; aluminium nitrate; chromium nitrate nonahydrate; ferric chloride hexahydrate; terephthalic acid; hydrofluoric acid; zinc nitrate hexahydrate; DMF yog tag nrho cov kev ntsuam xyuas hauv tsev. TU-1901 UV-pom spectrophotometer, Beijing Puxi General Instrument Co., Ltd.; XRD-6000X-ray diffractometer, Shimadzu Corporation, Nyiv; Hitachi S4800 txias teb emission scanning electron microscope, HITACHI Corporation, Nyiv; FTIR-650 Fourier transform infrared spectrometer, Beijing Puxi General Instrument Co., Ltd.; SDT Q600 thermogravimetric analyzer, TA Corporation, USA;

1.2 Synthesis of MOF cov ntaub ntawv

1.2.1 Synthesis of nicotinate zinc coordination polymer [Zn(nicotinate)2]n([Zn(NA)2])

Txoj kev siv [28], hnyav 2.336 g (8.14 mmol) ZnSO4∙7H2O, ntxiv 15 mL deionized dej, thiab yaj los ntawm ultrasonic. Noj 1. . Lim cov khoom, ntxuav nrog dej deionized thiab kub ethanol tov, thiab qhuav ntawm 150 degree rau 12 h kom tau [Zn(NA)2] ua cov khoom dawb.

1.2.2 Synthesis of MIL-101(Fe)

Xa mus rau [29], raug hnyav 1.350 g (0.024 mol) ntawm ferric chloride hexahydrate thiab 0.412 g (2.45 mmol) ntawm terephthalic acid, ntxiv 30 m DMF, do rau 30 min rau yaj, reactor nyob rau hauv ib tug hydrothermal reactor ntawm 110 degree rau 20 h, txias lawm, ntxuav cov khoom nrog DMF, purify nws ob zaug nrog 70 degree kub ethanol tov, txhua zaus rau 2 h, thiab qhuav cov khoom purified ntawm 150 degree rau 8 h. kom tau ib tug reddish xim av khoom hmoov.

1.2.3 Synthesis of MIL-101 (Cr)

Ua kom raug hnyav 2.699 g (16.06 mmol) ntawm terephthalic acid, 1.101 g (2.75 mmol) ntawm cadmium nitrate nonahydrate thiab 100 µL ntawm hydrofluoric acid, ntxiv rau hauv 30 mL ntawm dej deionized thiab do rau 30 feeb kom tau txais ib qho kev daws teeb meem. Hloov nws mus rau lub reactor thiab khaws cia ntawm 220 degree rau 8 h, txias nws ib txwm, lim thiab ntxuav cov khoom, thiab ziab nws hauv qhov cub ntawm 150 degree thaum hmo ntuj [30] kom tau cov hmoov grey-ntsuab.

1.2.4 Synthesis of MOF-5

Ua kom raug hnyav 0.356 g (2.12 mmol) ntawm terephthalic acid thiab 1.662 g (5.60 mmol) ntawm zinc nitrate hexahydrate, ntxiv 40 mL ntawm DMF thiab do cov tshuaj kom txog thaum nws pom tseeb, hnov ​​​​mob hauv autoclave ntawm 130 degree. rau 4 h, txias lawm, ntxuav nrog DMF ob peb zaug, hloov nrog dichloromethane rau 12 h kom tau cov hmoov dawb, qhuav thiab qhib cov qauv ntawm 160 degree rau kev siv tom qab [31-32].

1.2.5 Synthesis of MIL-53 (Fe)

Qhov hnyav {{0}}.473 g (1.75 mmol) ntawm ferric chloride hexahydrate thiab 0.291 g (1.73 mmol) ntawm terephthalic acid thiab yaj lawv nyob rau hauv 38 mL ntawm DMF, hnov ​​nyob rau hauv ib tug autoclave ntawm 170 degree rau 15 h. , txias lawm, thiab ntxuav nrog DMF hnyav ob peb zaug kom tau ib lub teeb txiv kab ntxwv hmoov khoom. Qhuav ntawm 150 degree rau 12 h [33].

1.3 Kev txiav txim siab ntawm tag nrho cov ntsiab lus flavonoid hauv cov qauv

1.3.1 Kev npaj ntawm rutin tus qauv nkhaus

Ua kom hnyav 10.0 mg ntawm rutin tus qauv qauv, yaj nws hauv 70% ethanol thiab dilute rau 100 mL los npaj ib { {15}}.100 mg∙mL-1 standard solution. Noj 0, 0.5, 1.0, 1.5, 2.0, 2.5, 3.0, 3.5, 4.0, 4.5 mL ntawm txheej txheem kev daws teeb meem, ntxiv 0.4 mL ntawm 5% NaNO2 tov, teb rau 6 min; tom qab ntawd ntxiv 0.4 mL ntawm 10% Al (NO3) 3 tov, rov ua dua rau 6 min; Tom qab ntawd ntxiv 4 mL ntawm 4% NaOH tov, dilute rau 10 ml volumetric hwj thiab cia sawv ntsug rau 15 feeb. Ntsuas qhov nqus ntawm 510 nm. Kev sib raug zoo ntawm absorbance A thiab rutin huab hwm coj concentration C tau tsim: C=0.08637A + 0.000701 (Daim duab 1), thiab qhov sib txheeb coefficient yog 0.9992, qhia tias rutin muaj kev sib raug zoo hauv qhov ntau ntawm 0 ~ 0.045 mg∙mL-1.

1.3.2 Kev txiav txim cov ntsiab lus piv txwv

Siv ib qho tsim nyog ntawm Cistanche deserticola hmoov coj mus kuaj thiab muab rho tawm nrog 70% ethanol tov ntawm 25 degree rau 2h raws li ib tug tej yam khoom-kua piv. Tom qab pom, tshem tawm ethanol los ntawm rotary evaporation thiab kho qhov ntim rau 250 mL. Siv 1 mL ntawm cov qauv kev daws teeb meem rau kev tsim xim thiab txiav txim siab nws qhov nqus. Cov ntsiab lus ntawm tag nrho cov flavonoids nyob rau hauv Cistanche deserticola yog xam los ntawm mis (1) [27]:

W=C × V × N / m (1) Qhov twg: V sawv cev rau lub ntim ntim ntawm cov qauv tshuaj, mL; W sawv cev rau tag nrho cov ntsiab lus flavonoid hauv cov qauv, mg∙g-1; C sawv cev rau qhov concentration ntawm flavonoids hauv cov qauv tshuaj, mg∙mL-1; m sawv cev rau cov qauv loj, g; N sawv cev rau dilution ntau.

Daim duab 1 Standard nkhaus ntawm Rutin

1.4 Static adsorption thiab desorption test ntawm tag nrho cov flavonoids hauv Cistanche deserticola los ntawm MOFs

1.4.1 Kev npaj ntawm crude extract ntawm tag nrho cov flavonoids nyob rau hauv Cistanche deserticola

Qhov hnyav 5 g ntawm Cistanche deserticola hmoov coj mus kuaj, ntxiv 150 mL ntawm 70% ethanol los ntawm ntim, rho tawm ntawm 60 degree rau 2 h, thiab tau txais cov khoom nyoos extract ntawm tag nrho cov flavonoids hauv Cistanche deserticola. Hauv qhov kev sim no, cov ntsiab lus ntawm tag nrho cov flavonoids hauv Cistanche deserticola yog 51.67 mg∙g-1, thiab purity yog 9.33%.

1.4.2 MOFs static adsorption thiab desorption test

Ua kom raug hnyav 100.0 mg ntawm txhua ntawm tsib MOFs cov ntaub ntawv thiab ntxiv rau 50 mL centrifuge raj, tom qab ntawd ntxiv 35 mL ntawm crude extract thiab ua ultrasonic dispersion. Adsorb rau 24 teev ntawm 150 r / min ntawm shaker ntawm 25 degree. Centrifuge tom qab adsorption thiab rho tawm 1 mL ntawm supernatant los txiav txim siab tag nrho cov ntsiab lus flavonoid, yog li xam tag nrho cov flavonoid adsorption tus nqi ntawm txhua MOF cov khoom.

Cov khoom siv MOF tom qab adsorption equilibrium yog ntxuav nrog dej deionized, thiab 20 mL ntawm desorption tov tau ntxiv. Cov khoom tau muab tso rau ntawm qhov ntsuas kub tsis tu ncua ntawm 25 degree thiab desorbed ntawm 150 r / min rau 24 teev. Centrifuge tom qab desorption thiab rho tawm 1 mL ntawm supernatant los txiav txim siab tag nrho cov ntsiab lus flavonoid hauv cov tshuaj desorption. Raws li cov kauj ruam saum toj no, qhov sib npaug adsorption tus nqi, tus nqi desorption thiab desorption tus nqi ntawm tsib MOFs cov ntaub ntawv rau tag nrho cov flavonoids tau xam [34]. Qe=(C0− Ce)×Vi/m (2)

Qd{0}}Cd × Vd/m (3)

Rd(%)=Qd/Qe × 100% (4)

Qhov twg: m sawv cev qhov hnyav ntawm MOFs, g; Qd sawv cev rau tus nqi desorption, mg∙g{{0}}; Qe sawv cev rau qhov sib npaug ntawm qhov nqus, mg∙g-1; Cd sawv cev rau qhov concentration ntawm cov tshuaj desorption, mg∙mL-1; Rd sawv cev rau tus nqi desorption, %; C0 sawv cev rau thawj zaug concentration ntawm cov tshuaj adsorption, mg∙mL-1; Ce sawv cev rau qhov sib npaug ntawm cov tshuaj adsorption, mg∙mL-1; Vd sawv cev rau qhov ntim ntawm cov tshuaj desorption, mL; Vi sawv cev rau qhov ntim ntawm cov qauv tshuaj, mL.

1.5 Kev txiav txim siab ntawm qhov zoo tshaj plaws adsorption tej yam kev mob ntawm [Zn(NA)2] ntawm Cistanche deserticola

1.5.1 Static adsorption kinetic nkhaus

Ua kom hnyav 1.0 g ntawm [Zn(NA)2] qauv, ntxiv 200 mL ntawm Cistanche deserticola crude extract, thiab adsorb rau ntawm shaker ntawm 25 degree thiab 150 r / min. Tshem tawm 1 mL ntawm supernatant rau kev soj ntsuam ntawm ib lub sijhawm luv los txiav txim siab cov ntsiab lus ntawm tag nrho cov flavonoids. Nyob rau tib lub sijhawm, txuas ntxiv ntxiv cov tshuaj tshiab kom txog thaum adsorption equilibrium.

1.5.2 Cov nyhuv ntawm adsorbent ntau npaum li cas ntawm adsorption ntawm tag nrho cov flavonoids hauv Cistanche deserticola

Ua kom raug hnyav 20, 60, 100, 140, 180, thiab 200 mg [Zn(NA)2], ntxiv 35 mL ntawm cov kua extract, thiab tom qab adsorption equilibrium, centrifuge thiab noj 1 mL ntawm supernatant rau kev tsom xam thiab kev txiav txim siab ntawm tag nrho cov ntsiab lus flavonoid. .

1.5.3 Kev sib raug zoo ntawm cov adsorption ntawm tag nrho cov flavonoids hauv Cistanche deserticola thiab thawj concentration ntawm cov qauv. Npaj cov qauv kev daws teeb meem ntawm crude flavonoid extract ntawm Cistanche deserticola nrog ntau ntawm 0.64, 1.28, 1.76, 2.20, 2.84, thiab 3.6 mg∙mL-1, ntxiv 100 mg [Zn(NA)2 ], adsorb rau 6 h, centrifuge thiab noj 1 mL ntawm supernatant rau kev tsom xam thiab kev txiav txim, thiab xam cov adsorption ntawm [Zn(NA)2] rau tag nrho cov flavonoids.

1.5.4 Kev sib raug zoo ntawm adsorption ntawm tag nrho cov flavonoids ntawm Cistanche deserticola thiab pH tus nqi ntawm cov qauv tshuaj

Qhov kev sim tau xaiv ib qho kev daws teeb meem nrog qhov concentration ntawm 2.20 mg∙mL-1, thiab kho tus nqi pH ntawm cov qauv tshuaj rau 3.0, 4.0 , 5.{{10}}, 6.0, 7.0, thiab 8.0. Tom qab 6 teev ntawm adsorption, lub adsorption mus txog lub xeev tiav, thiab 1 mL ntawm supernatant tau centrifuged rau kev tshuaj xyuas. Tom qab ntawd cov adsorption ntawm [Zn(NA)2] ntawm tag nrho cov flavonoids raug xam.

1.6 Kev txiav txim siab ntawm qhov zoo tshaj plaws desorption tej yam kev mob ntawm [Zn(NA)2] ntawm Cistanche deserticola

1.6.1 Cov nyhuv ntawm desorption kev ua tau zoo thiab cov kev daws teeb meem sib txawv desorption

Rau oscillation desorption ntawm [Zn(NA)2] ntawm adsorption equilibrium, cov nyhuv ntawm kev xaiv ethanol, n-butanol, methanol, thiab ethyl acetate raws li desorption daws ntawm desorption kev ua tau zoo ntawm [Zn(NA)2] raug soj ntsuam.

1.6.2 Cov nyhuv desorption ntawm ethanol concentration

[Zn(NA)2] ntawm adsorption equilibrium desorbed, thiab cov nyhuv ntawm ethanol aqueous tov nrog desorption kua ntim feem ntawm 10%, 30%, 50%, 70%, thiab 90% ntawm desorption nyhuv ntawm [Zn(NA) 2] tau kawm. Qhov zoo tshaj plaws analytical tej yam kev mob raug txiav txim.

1.5.2 Cov nyhuv ntawm adsorbent ntau npaum li cas ntawm adsorption ntawm tag nrho cov flavonoids hauv Cistanche deserticola

Ua kom raug hnyav 20, 60, 100, 140, 180, thiab 200 mg [Zn(NA)2], ntxiv 35 mL ntawm cov kua extract, thiab tom qab adsorption equilibrium, centrifuge thiab noj 1 mL ntawm supernatant rau kev tsom xam thiab kev txiav txim siab ntawm tag nrho cov ntsiab lus flavonoid. .

1.5.3 Kev sib raug zoo ntawm cov adsorption ntawm tag nrho cov flavonoids hauv Cistanche deserticola thiab thawj concentration ntawm cov qauv. Npaj cov qauv kev daws teeb meem ntawm crude flavonoid extract ntawm Cistanche deserticola nrog ntau ntawm 0.64, 1.28, 1.76, 2.20, 2.84, thiab 3.6 mg∙mL-1, ntxiv 100 mg [Zn(NA)2 ], adsorb rau 6 h, centrifuge thiab noj 1 mL ntawm supernatant rau kev tsom xam thiab kev txiav txim, thiab xam cov adsorption ntawm [Zn(NA)2] rau tag nrho cov flavonoids.

1.5.4 Kev sib raug zoo ntawm adsorption ntawm tag nrho cov flavonoids ntawm Cistanche deserticola thiab pH tus nqi ntawm cov qauv tshuaj

Qhov kev sim tau xaiv ib qho kev daws teeb meem nrog qhov concentration ntawm 2.20 mg∙mL-1, thiab kho tus nqi pH ntawm cov qauv tshuaj rau 3.0, 4.0 , 5.{{10}}, 6.0, 7.0, thiab 8.0. Tom qab 6 teev ntawm adsorption, lub adsorption mus txog lub xeev tiav, thiab 1 mL ntawm supernatant tau centrifuged rau kev tshuaj xyuas. Tom qab ntawd cov adsorption ntawm [Zn(NA)2] ntawm tag nrho cov flavonoids raug xam.

1.6 Kev txiav txim siab ntawm qhov zoo tshaj plaws desorption tej yam kev mob ntawm [Zn(NA)2] ntawm Cistanche deserticola

1.6.1 Cov nyhuv ntawm desorption kev ua tau zoo thiab cov kev daws teeb meem sib txawv desorption

Rau oscillation desorption ntawm [Zn(NA)2] ntawm adsorption equilibrium, cov nyhuv ntawm kev xaiv ethanol, n-butanol, methanol, thiab ethyl acetate raws li desorption daws ntawm desorption kev ua tau zoo ntawm [Zn(NA)2] raug soj ntsuam.

1.6.2 Cov nyhuv desorption ntawm ethanol concentration

[Zn(NA)2] ntawm adsorption equilibrium desorbed, thiab cov nyhuv ntawm ethanol aqueous tov nrog desorption kua ntim feem ntawm 10%, 30%, 50%, 70%, thiab 90% ntawm desorption nyhuv ntawm [Zn(NA) 2] tau kawm. Qhov zoo tshaj plaws analytical tej yam kev mob raug txiav txim.