ICP-MS txiav txim siab cov ntsiab lus ntawm ntau yam kab hauv Cistanche Deserticola los ntawm txawv keeb kwm

Abstract:

Lub Hom Phiaj:Txhawm rau tsim kom muaj microwave digestion-inductively coupled plasma mass spectrometry (ICP-MS) txoj kev txiav txim siab rau 37 lub ntsiab lus, txhawm rau txheeb xyuas thiab txheeb xyuas 37 cov ntsiab lus inorganic hauvCistanche deserticolalos ntawm txawv keeb kwm, thiab ua ntej tshawb nrhiav thiab kawm txog ntau yam inorganic ntsiab nyob rau hauvCistanche deserticolalos ntawm txawv keeb kwm. kev faib tawm ntawm cov pa phem.

Cov txheej txheemNitric acid-hydrogen peroxide tau siv los ua kev zom zaub mov, thiab txoj kev zom zaub mov microwave tau siv los ua tus qauv ua ntej. Cov ntsiab lus ntawm 37 inorganic ntsiab nyob rau hauvCistanche deserticolatau txiav txim siab ib txhij los ntawm kev siv cov txheej txheem sab hauv hauv online calibration thiab lwm tus qauv quantitative ICP-MS txoj kev. Cov txiaj ntsig tau pom muaj kev sib raug zoo nrog thaj chaw ncov (r Ntau dua lossis sib npaug rau 0.0.997 4) hauv qhov nkhaus ntawm 0.{{5 }}.50 to 1{{10}}0 ug·L-1 (Hg: 0.0.20 to 20 ug·L{ {13}}), thiab qhov kev txwv tsis pub tshaj yog 0.000 27 ~ 0.045 ug·L-1, tus txheej txheem rov qab yog nyob ntawm peb theem ntxiv ntawm siab, nruab nrab thiab qis. Qhov nruab nrab rov qab tus nqi ntawm lub caij yog nyob nruab nrab ntawm 76.5% thiab 110.0%. Qhov ntsuas precision yog Thetxheeb ze tus qauv sib txawv(RSD) qhov tseem ceeb thiab rov ua dua tau tag nrho <4.8%; Kev tshawb pom ntawm 5 teeb meem hlau hnyav (tooj liab, txhuas, arsenic, mercury, cadmium) hauv 40 pawg ntawmCistanche deserticolatias 2020 tsab ntawm "Suav Pharmacopoeia" kom meej meej yuav tsum tau tswj xyuas cov nqi ntawm barium caij, manganese caij, rubidium caij thiab strontium caij hauv 40 pawg ntawm cov qauv yog tag nrho 100%, thiab lawv cov ntsiab lus nyob deb ntawm ib leeg. Ntau dua li lwm cov ntsiab lus, nrog pom tseeb hauv cheeb tsam sib txawv. .

Xaus:Cov txheej txheem no muaj qhov rhiab heev thiab zoo rov tsim dua tshiab, txo lub sijhawm tshuaj xyuas, thiab txo cov nqi tshuaj xyuas. Nws tuaj yeem tshawb xyuas ntau yam khoom tsis zoo hauv Cistanche deserticola tib lub sijhawm thiab muab cov ntaub ntawv txhawb nqa rau kev cog qoob loo zoo ntawm Cistanche deserticola thiab ua kom cov khoom siv tshuaj zoo thiab kev nyab xeeb ntawm cov tshuaj.

Ntsiab lus:Cistanche deserticola; inorganic ntsiab; microwave digestion; inductively txuas plasma huab hwm coj spectrometry

Organic CISTANCHE EXTRACT nrog 30% ECHINACOSIDE thiab 12% ACTEOSIDE

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Cov nroj tsuag ntawm genus Cistanche yog perennial obligate cag cab kab mob ntawm cov nroj tsuagtsev neeg Orobanceae, tseem hu ua loj rhizome, gnome, golden xyoob tua, thiab lwm yam. 1]

Muaj 4 hom thiab 1 ntau yamCistanche deserticola nroj tsuaghauv kuv lub tebchaws, suav nrog suab puam Cistanche deserticola, tubular pajCistanche deserticola, ntsev cistanche, dawb-flowered ntsev cistanche, thiab xuab zeb suab puam cistanche. Cistanche deserticola tau sau tseg hauv xyoo 2020 tsab ntawm "Suav Pharmacopoeia" yog cov qia qhuav ntawm cov suab puam Cistanche deserticola thiab tubular paj Cistanche deserticola. Cistanche deserticola yog kab mob parasitic ntawm cov hauv paus hniav ntawm genus Tamarix nyob rau hauv cov suab puam thiab feem ntau yog faib nyob rau hauv cov suab puam thaj tsam ntawm yav qab teb Xinjiang. Suab puam Cistanche deserticola yog kab mob cab rau ntawm cov hauv paus hniav ntawm cov xuab zeb kho cua daj cua dub cog Haloxylon ammodendron thiab feem ntau yog muab faib rau hauv thaj chaw suab puam xws li Alxa League (Sab laug Banner, Txoj Cai Banner, Ejina Banner), Gansu thiab sab qaum teb Xinjiang hauv Inner Mongolia [{{3] }}].

ECHINACOSIDE thiab ACTEOSIDE

Cov ntsiab lus inorganic ua lub luag haujlwm tseem ceeb hauv tag nrho kev loj hlob ntawm cov nroj tsuag. Vim muaj kev cuam tshuam ntawm cheeb tsam thiab ib puag ncig kev loj hlob, cov seem ntawm cov khoom inorganic hauv cov nroj tsuag kuj txawv. Rau tib neeg lub cev, thaum lawv nyob rau hauv lub feem ntau haum concentration range Tsuas yog ces tib neeg lub cev yuav nyob rau hauv ib tug noj qab nyob zoo lub xeev. Qee cov ntsiab lus inorganic yog exogenous teeb meem, xws li txhuas, cadmium, chromium, arsenic thiab mercury thiab lwm yam inorganic hlau, uas yog ib qho tseem ceeb cov pa phem nyob rau hauv tsoos suav tshuaj; Kuj tseem muaj qee cov kab mob uas tsim nyog rau tib neeg lub cev, xws li tooj liab, hlau, zinc, thiab lwm yam. Thaum nws accumulates mus rau ib qho concentration hauv tib neeg lub cev, nws yuav rhuav tshem qhov sib npaug thiab ua rau muaj kev hloov pauv pathological [{{0} }].

Cistanche deserticola yog ob qho tib si cov khoom siv tshuaj thiab cov khoom noj khoom haus, yog li nws cov khoom sib xyaw ntawm cov khoom siv tsis zoo yuav tsum nyiam mloog. Nws yog ib qho tsim nyog los xyuas thiab txheeb xyuas cov ntsiab lus ntawm ntau yam inorganic ntsiab. Raws li cov lus qhia dav dav ntawm Suav Pharmacopoeia, tus sau tau siv microwave digestion-inductively coupled plasma mass spectrometry (ICP-MS) ib txhij ntsuas 37 inorganic ntsiab hauv Cistanche deserticola. Los ntawm kev txheeb xyuas cov ntaub ntawv xeem, tus sau tau muab lub hauv paus rau kev cog qoob loo zoo thiab kev lees paub zoo ntawm Cistanche deserticola. thiab muab cov ntaub ntawv txhawb kev nyab xeeb ntawm tshuaj.

1 Reagents thiab ntsuas

1.1 Kev ntsuas

Shimadzu 2030 inductively coupled plasma mass spectrometer (Shimadzu, Nyiv); Multiwater 7000 microwave digestion instrument (Anton Paar, Austria); ME204 hluav taws xob tshuav nyiaj li cas (Mettler, Switzerland). Milli⁃Q ultrapure dej ntsuas (Millipore Corporation, USA).

1.2 Reagents

Cov txheej txheem sib xyaw ua ke ntawm 36 cov ntsiab lus suav nrog lithium (ntau cov ntsiab lus: 10 ug·mL-1); mercury ib qho txheej txheem daws teeb meem (ntau npaum li cas: 1000 ug·mL-1); rhenium (Re) cov txheej txheem kev daws teeb meem sab hauv (ntau cov ntsiab lus: 1 000 ug·mL-1); rhodium (Rh) cov txheej txheem kev daws teeb meem (ntau npaum li cas: 1000 ug·mL-1, Agilent); ultrapure dej (resistivity 18.12 MΩ·cm) ua hauv chav kuaj; nitric acid (68.0%-70.0%, UPS qib), hydrogen peroxide (30.0%-32.0%, UPS qib) (Suzhou Jingrui Chemical Co., Ltd.).

1.3 Test qauv

40 batch ntawm Cistanche deserticola cov ntaub ntawv tshuaj thiab daim ntawv sau los ntawm ntau yam khoom siv tshuaj ntau lawm

Cov tuam txhab lag luam, khw muag tshuaj thiab cov khoom muag tus kheej tau tsim hauv Xinjiang, Gansu thiab Inner Mongolia feem. Lawv tau lees paub los ntawm Song Pingshun, tus kws muag tshuaj ntawm Gansu Provincial Institute for Drug Inspection. Cov qauv sau tau raug muab tshem tawm los ntawm cov impurities xws li sediment thiab qhuav ua ntej siv.

2 Cov txheej txheem thiab cov txiaj ntsig

2.1 Kev npaj cov txheej txheem kev daws teeb meem

Ntsuas ntsuas cov txheej txheem sib xyaw ntawm 36 cov ntsiab lus suav nrog lithium (10mg·L-1

), dilute nws nrog 2% nitric acid aqueous tov los npaj cov txheej txheem sib xyaw ua ke ntawm 36 cov ntsiab lus xws li lithium nrog qhov loj ntawm 1000 ug·L-1, thiab khaws cia rau hauv -5 degree txias txias txias; ntsuas qhov ntsuas mercury tib lub ntsiab Standard tov (1 000 mg·L-1

), ntxiv qhov tsim nyog ntawm nitric acid aqueous tov nrog ib feem ntawm 2% rau dilute nws los npaj cov mercury ib yam khoom txheem txheej txheem tov nrog ib tug loj concentration ntawm 100 ug·L-1, uas yuav tsum tau npaj. tam sim ntawd.

2. 2 Kev npaj cov txheej txheem sab hauv

Precisely ntsuas qhov tsim nyog ntawm Re internal standard tov thiab Rh internal standard tov, ntxiv 2% ntim feem ntawm nitric acid aqueous tov rau dilute thiab npaj ib tug tov nrog cov txheej txheem tov nrog ib tug loj concentration ntawm 500 ug·L-1.

2.3 Kev npaj cov tshuaj ntsuam xyuas

Precisely hnyav txog 0.3 g ntawm Cistanche deserticola qauv hmoov (dhau los ntawm No. 3 sieve) thiab muab tso rau hauv ib lub tank zom. Ntxiv 2 mL ntawm nitric acid thiab 1 mL dej ultrapure thiab cia nws sawv ntsug ib hmos. Hnub tom qab, ntxiv 1 mL ntawm hydrogen peroxide thiab muab tso rau hauv lub plab zom mov. Digest nyob rau hauv microwave digestion cub (saib Table 1 rau cov txheej txheem digestion). Tom qab digestion tiav, tshem tawm

Lub plab zom mov tau muab tso rau ntawm lub phaj hluav taws xob cua sov (kub qis dua 100 degree) thiab ua kom sov maj mam. Tom qab cov xim liab-xim av hauv lub plab zom mov tau evaporated, nws tuaj yeem raug tshem tawm thiab tso cai rau txias rau chav tsev kub. Cov tshuaj digestion yog pauv mus rau 50 mL ntsuas lub raj mis nrog dej ultrapure ob peb zaug. , siv ultrapure dej los kho qhov ntim rau lub cim, thiab siv tib txoj kev los ua ib qho qauv dawb rau kev ntsuas ICP-MS.

2. 4 ICP⁃Ｓ Kev khiav hauj lwm tej yam kev mob

Lub zog RF yog 1550 W, qhov kub ntawm cov tshuaj tsuag chamber yog 5 degree, nws yog kev sib tsoo cov tshuaj tiv thaiv, qhov ntsuas qhov tob yog 5. . qauv yog ntsuas 3 zaug kom tau txais tus nqi nruab nrab. Thaum lub sij hawm soj ntsuam cov txheej txheem, txhawm rau kho thiab them nyiaj rau cov nyhuv matrix thiab cov teeb liab drift ntawm cov qauv, Re thiab Rh tau raug xaiv los ua cov qauv hauv online yam tsis muaj kev cuam tshuam rau cov ntsiab lus ntsuas.

2.5 Linear ntau yam, nrhiav kom pom kev txwv thiab txwv kom muaj nuj nqis

Qhov tseeb ntsuas 36 cov txheej txheem sib xyaw ua ke ntawm lithium thiab lwm yam khoom siv 005, 01, {{10}}}05, 1 .0, 5.0, 1{{20}}. {32}}}}20, 0.50, 1.0 , 2.0, 5.0, 20. Npaj 36 yam ntawm cov txheej txheem sib xyaw ua ke xws li 0.50, 1.00, 5.0.0, 10.0.0, 50.0.0, 100.0 .0 ug·L-1 lithium thiab lwm cov txheej txheem sib xyaw ua ke thiab 0.0.20, 0.0.50, 1. 0, 2 0, 50, 200 0 ug·L{{ 58}} mercury ib qho txheej txheem txheej txheem daws teeb meem, npaj ua rau siv ib ntus.

Kho ICP-MS rau qhov kev ua haujlwm zoo tshaj plaws, ntsuas cov txheej txheem kev daws teeb meem nkhaus, ua cov kab rov qab ntawm nws qhov loj nrog nws cov lus teb tus nqi, thiab tau txais cov kab zauv sib npaug. Cov txiaj ntsig tau pom tias cov lus teb tus nqi ntawm cov ntsiab lus ntsuas yog nyob ntawm qhov loj ntawm 0.50 txog 100 ug·L-1 (Hg:Txoj kev sib raug zoo yog qhov zoo nyob rau hauv thaj tsam ntawm {{0}}.20 txog 20 ug·L-1), thiab cov coefficients sib raug zoo tag nrho ntau dua 0.997 4, qhia tias nyob rau hauv no loj concentration ntau, qhov ntsuas teb ntawm lub ntsuas ntsuas yog linear nrog nws loj concentration. Qhov kev kuaj xyuas qhov txwv thiab kev txwv qhov txwv txiav txim siab txiav txim siab los ntawm qhov ntsuas tom qab tus qauv nkhaus tiav.

tau muab, thiab cov txiaj ntsig tau qhia hauv Table 2.