Kev txiav txim ib txhij ntawm Echinacoside Thiab 2,3,5,4'-tetrahydroxy Stilbene-2-Ο- -D-glucoside hauv Congrong Tongbian Oral Liquid Los ntawm HPLC

Abstract:Lub hom phiaj yog los txiav txim siab echinacoside ib txhij thiab 2,3,5,4'-tetrahydroxy stilbene-2-Ο- -D-glucoside hauv Congrong digestive qhov ncauj kua los ntawmHPLC. Tech Mate C18-ST (4.6 mm × 25{12}} 0 mm, 5 μm) kem tau siv nrog gradientelution los ntawm acetonitrile-0.2% formic acid kua; qhov ntsuas wavelength yog 330nm; tus nqi ntws yog 1.0 mL/min. Cov txiaj ntsig tau pom tias echinacoside thiab 2,3,5,4'-tetrahydroxy stilbene-2-Ο- -D-glucoside hauv cov qauv nthuav tawm qhov kev daws teeb meem zoo los ntawm cov chromatographic peaks uas nyob ib sab nrog kev sib raug zoo linear hauv thaj tsam ntawm 0 .159 3-0.955 8 ug and 0.385 3-4 {32}} ug. Txoj kev tsim yog yooj yim thiab raug thiab siv tau los txiav txim echinacoside andstilbene glycoside hauv Congrong digestive qhov ncauj kua.

Ntsiab lus:Congrong Degestive qhov ncauj kua;echinacoside cov tshuaj; 2,3,5,4'-tetrahydroxystilbene-2-Ο- -D-glucoside; HPLC

ORGANIC CISTANCHE EXTRACT nrog 30% ECHINACOSIDE thiab 12% ACTEOSIDE

Cov qauv zoo tam sim no ntawmCistanche Rongdigestive Oral Liquid muaj teeb meem xws li cov khoom sim yooj yim, kev ua haujlwm tsis zoo, thiab kev ua haujlwm nyuaj thiab siv sijhawm ntev. Ntxiv nrog rau cov khoom kuaj xyuas dav dav, tus qauv tsuas yog muaj cov txheej txheem nyias nyias rau Polygonum multiflorum thiab Citrus aurantium, thiab Polygonum multiflorum thiab Citrus aurantium. Qhov tseeb nyias txheej chromatography qhia txog txoj kev tsis nruj txaus thiab muaj kev ua haujlwm tsis zoo. Cov ntsiab lus txiav txim siab siv ultraviolet spectrophotometry los kuaj 1,8-dihydroxyanthraquinone hauv Cistanche purpurea kua qhov ncauj. Txij li txoj kev no yuav tsum muaj ntau yam reflux extractions, Lub lag luam yog cumbersome thiab siv sij hawm, thiab cov reproductibility thiab raug yog tsis zoo. Qhov zoo ntawm cov khoom siv tshuaj qub tsis tuaj yeem tswj tau, thiab kev tswj hwm ntawm huab tais cov tshuaj Cistanche deserticola tsis muaj. Nyob rau hauv no standard kev tshawb fawb ua hauj lwm, kev txiav txim ntawmechinaceaside hauv Cistanche deserticolathiabStilbene glycoside nyob rau hauv Polygonum multiflorumHauv Cistanche deserticola Oral Liquid tau kawm. Raws li cov qauv kev muaj pes tsawg leeg thiab cov txheej txheem cov yam ntxwv, ib theem ua kua ua tau zoo tau tsim. Cov txheej txheem chromatographic tau siv los txiav txim siab echinacoside thiab stilbene glycosides hauv Cistanche Rong digestive Oral Liquid, thiab nws cov ntsiab lus txwv tau tsim los txhawm rau txhim kho thiab txhim kho cov qauv tswj kom zoo. Txoj kev txiav txim siab yog yooj yim thiab ceev, thiab cov ntsiab lus txwv yog tsim nyog. Tom qab kev txheeb xyuas cov txheej txheem, qhov tseeb, precision, linearity, durability, thiab ntau qhov tseeb yog qhov zoo, thiab lawv tuaj yeem siv los txiav txim siab cov ntsiab lus ntawm Cistanche Rong Tongbang Oral Liquid [1-5].

1 Cov cuab yeej thiab cov tshuaj reagents

1.1 Cov cuab yeej

Cov dej ua haujlwm siab ua kua chromatograph (2695 thiab ARC); 1/100,000 tshuav nqi hluav taws xob (MS205DU), 1/10,000 hluav taws xob tshuav (ME204E, Mettler-Toledo).

1.2 Xeem tshuaj thiab tshuaj reagents

Echinacea sab (batch tooj 110670-201706, purity 89.7%); stilbene glycoside (batch tooj 110844-201915, purity 90.7%), tag nrho yog muab los ntawm Tuam Tshoj lub koom haum ntawm Food and Drug Control; Cistanche purpurea cov kua hauv qhov ncauj (batch naj npawb 20191204, 20191205, 20191206, 20200404, 20200405, 20200406, 20200407, 20200408, 2020104020, G nws; methanol, thiab lwm yam yog chromatographically ntshiab; dej yog ultrapure dej; Lwm cov reagents yog qib ntsuas.

2 Cov txheej txheem thiab cov txiaj ntsig

2.1 Chromatographic tej yam kev mob

Siv Tech Mate C{{0}}ST (4.6 mm × 250. 0.2% formic acid tov raws li theem mobile B. Ua gradient elution raws li cov kev cai nyob rau hauv Table 1; kem kub Qhov kub yog 35 degree; Kev tshawb pom wavelength yog 330 nm; tus nqi ntws yog 1.0 mL / min; qhov ntim ntawm cov qauv kuaj thiab cov khoom siv yog 10 µL txhua; tus naj npawb ntawm cov phiaj xwm theoretical yuav tsum tsis pub tsawg dua 4000 raws li lub ncov echinaceaside.

2.2 Kev npaj kev daws teeb meem

Kev npaj cov tshuaj siv: Siv cov khoom siv echinaceaside thiab stilbene glycoside siv cov khoom tsim nyog, ntsuas lawv kom raug, thiab ntxiv 70% methanol los npaj cov tshuaj tov uas muaj 7{10}} ug ntawm echinaceaside thiab 150 ug. stilbene glycoside ib 1 mL. , yog nws. Kev npaj ntawm cov tshuaj ntsuam xyuas: Co cov khoom kom zoo, noj li 0.3 g, hnyav kom raug, muab tso rau hauv 25 mL xim av ntsuas lub raj mis, ntxiv ib qho tsim nyog tus nqi ntawm 70% methanol, sonicate rau 30 feeb, cia nws txias, ntxiv 70 % methanol rau dilute rau Scale, co zoo, lim, thiab coj cov seem filtrate kom tau. Kev npaj cov qauv tsis zoo: Precisely hnyav txog 0.3 g ntawm cov qauv tsis zoo thiab npaj nws raws li kev npaj ntawm cov tshuaj ntsuam xyuas.

Daim duab 1 HPLC chromatograms ntawm Congrong digestive qhov ncauj kua

2.3 Methodological tshuaj xyuas

2.3.1 Ua haujlwm nkhaus thiab linear ntau yam

Precisely kos cov lus sib xyaw ua ke thiab ntxiv 70% methanol los npaj cov kev daws teeb meem sib xyaw. Precisely kos 1{{20}} µL ntawm txhua qhov saum toj no series ntawm kev tswj kev daws teeb meem, txhaj rau hauv cov kua chromatograph, thiab ntsuas qhov chaw siab tshaj qhov sib xyaw ua ke. Siv qhov concentration ntawm kev siv tshuaj (µg/mL) raws li qhov ordinate (x) thiab thaj chaw ncov sib xyaw ua ke raws li abscissa (y). Kos ib daim duab kom tau ib txoj kab ncaj nraim hla lub hauv paus chiv keeb. Qhov sib npaug regression yog y1=1. } . Cov txiaj ntsig tau pom tias echinaceaside thiab stilbene glycoside muaj kev sib raug zoo linear hauv qhov ntau ntawm 0.159 3 txog 0.955 8 ug thiab 0.385 3 txog 4.623 5 ua ug.

Cistanche Tubulosa

2.3.2 Precision xeem

Precisely kos 10 µL ntawm cov tshuaj sib xyaw ua ke, thiab rov txhaj tshuaj 6 zaug raws li "2.1" chromatographic mob. RSD ntawm thaj chaw ncov ntawm echinacoside thiab stilbene glycoside raug ntsuas los ntawm 0.66% thiab 0.59% raws li, qhia tias qhov ntsuas qhov ntsuas tau zoo.

2.3.3 Stability test

Raws li txoj kev hauv qab "2.1", coj cov khoom no (batch naj npawb 20191205) los ua cov tshuaj ntsuam xyuas, txhaj cov qauv rau kev ntsuas ntawm 0 h, 4 h, 8 h, 12 h, 20 h, thiab 24 teev tom qab kev npaj, thiab sau qhov chaw siab tshaj. , tus txheeb ze tus qauv sib txawv ntawm 2.37% thiab 2.79%. Cov txiaj ntsig tau pom tias cov tshuaj ntsuam xyuas ruaj khov hauv 24 teev.

2.3.4 Repeatability test

Siv 6 aliquots ntawm tib batch ntawm cov qauv kuaj (batch naj npawb 20191205) thiab txhaj cov qauv rau kev ntsuas raws li chromatographic tej yam kev mob nyob rau hauv "2.1". Cov txiaj ntsig Tus txheeb ze tus qauv sib txawv ntawm echinaceaside yog 1.48%, nrog kev rov ua tau zoo; tus txheeb ze tus qauv sib txawv ntawm stilbene glycoside yog 1.10%, nrog zoo rov ua dua.

Cistanche Tubulosa

2.3.5 Kev txiav txim siab rov qab

Txais coj mus kuaj ntxiv thiab rov qab los muab 50% ntawm tus nqi piv txwv (0.3 g) ntawm cov qauv xeem thiab cov ntsiab lus piv txwv ntawm 1.0:0 .5, 1.{{10}}:1.0, 1. 0.431 5 mg/mL) 1. huab hwm coj concentration 0.8678 mg/mL) 1.25 mL, 2.50 mL, thiab 3.75 mL feem. Ntxiv rau 25 mL volumetric flasks feem, siv

Tshuab ziab khaub ncaws nrog nitrogen blower. Tom qab ntawd ua kom raug hnyav 9 cov qauv ntawm tib pawg nrog cov ntsiab lus paub (batch tooj 20191205, echinaceaside cov ntsiab lus yog 7.810 2 mg/g, stilbene glycoside cov ntsiab lus yog 14.232 4 mg/ g), thiab tus nqi piv txwv ntawm txhua tus qauv yog Tus qauv tus nqi ntawm cov qauv kuaj yog kwv yees li 0.15 g. Ntxiv nws rau saum lub khob ntim dej raws li. Npaj nws raws li txoj kev nyob rau hauv qhov kev xeem daws. Ntsuas raws li txoj cai. Xam tus nqi rov qab. Qhov tshwm sim yog ib qho yooj yim.

Qhov nruab nrab rov qab los ntawm stilbene glycosides thiab stilbene glycosides yog 98.28% thiab 98.43%, feem, thiab RSDs yog 1.56% thiab 0.97%, ntsig txog, qhia qhov ntsuas qhov tseeb.

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