Abstract
9,10-Anthraquinone (AQ) yog cov kab mob uas muaj peev xwm ua rau mob qog noj ntshav thiab tshwm sim hauv tshuaj yej thoob ntiaj teb. Qhov siab tshaj plaws residue txwv (MRL) ntawm AQ hauv tshuaj yej teeb los ntawm European Union (EU) yog 0.02 mg / kg. Cov peev txheej ntawm AQ hauv kev ua tshuaj yej thiab cov theem tseem ceeb ntawm nws qhov tshwm sim tau tshawb xyuas raws li kev hloov kho AQ analytical method thiab gas chromatography-tandem mass spectrometry (GC-MS/MS) tsom xam. Piv nrog rau hluav taws xob raws li qhov kub ntawm cov tshuaj yej ntsuab ua, AQ nce 4.3 mus rau 23.9 npaug ntawm cov tshuaj yej ua nrog cov thee raws li qhov chaw tshav kub, deb tshaj 0.02 mg / kg, thaum AQ theem nyob rau hauv ib puag ncig tripled. Tib yam tau pom nyob rau hauv oolong tshuaj yej ua nyob rau hauv thee tshav kub. Cov kauj ruam nrog kev sib cuag ncaj qha ntawm cov tshuaj yej nplooj thiab fumes, xws li fixation thiab ziab, yog suav tias yog cov kauj ruam tseem ceeb ntawm AQ ntau lawm hauv tshuaj yej ua. Cov theem ntawm AQ nce ntxiv nrog lub sijhawm sib cuag, qhia tias muaj kuab paug siab AQ hauv tshuaj yej tuaj yeem tau txais los ntawm cov pa taws los ntawm cov thee thiab combustion. Plaub caug cov qauv los ntawm kev cob qhia sib txawv nrog hluav taws xob lossis thee raws li cov khoom siv hluav taws xob tau txheeb xyuas, thaj tsam ntawm 50.0% -85.0% thiab 5.0% -35.0% rau kev kuaj pom thiab tshaj tus nqi ntawm AQ. Tsis tas li ntawd, qhov siab tshaj plaws AQ cov ntsiab lus ntawm 0.064 mg / kg tau pom nyob rau hauv cov tshuaj yej cov khoom nrog thee raws li lub tshav kub qhov chaw, qhia tau hais tias cov theem siab ntawm AQ paug nyob rau hauv cov tshuaj yej cov khoom yog feem ntau yuav pab tau los ntawm thee.
Cov ntsiab lus tseem ceeb: 9,10-Anthraquinone, Tshuaj yej ua, Coal, Qhov chaw paug
Taw qhia
Tshuaj yej tsim los ntawm nplooj ntawm evergreen shrub Camellia sinensis (L.) O. Kuntze, yog ib qho ntawm cov dej haus nrov tshaj plaws hauv ntiaj teb vim nws cov saj thiab cov txiaj ntsig kev noj qab haus huv. Hauv 2020 thoob ntiaj teb, tshuaj yej ntau lawm tau nce mus rau 5,972 lab metric tons, uas yog ob npaug hauv 20 xyoo dhau los[1]. Raws li kev sib txawv ntawm kev ua, muaj rau hom tshuaj yej tseem ceeb, suav nrog tshuaj yej ntsuab, tshuaj yej dub, tshuaj yej tsaus, tshuaj yej oolong, tshuaj yej dawb thiab tshuaj yej daj [2,3]. Txhawm rau kom ntseeg tau qhov zoo thiab kev nyab xeeb ntawm cov khoom, nws yog ib qho tseem ceeb heev uas yuav tsum tau saib xyuas cov theem ntawm cov pa phem thiab txhais lub hauv paus chiv keeb.

Kev txheeb xyuas qhov chaw ntawm cov khoom paug, xws li cov tshuaj tua kab, cov hlau hnyav thiab lwm cov pa phem xws li polycyclic aromatic hydrocarbons (PAHs), yog thawj kauj ruam los tswj cov pa phem. Kev txau ncaj qha ntawm cov tshuaj hluavtaws hauv cov tshuaj yej cog, nrog rau huab cua drift tshwm sim los ntawm kev ua haujlwm ze ntawm lub vaj tshuaj yej, yog lub hauv paus tseem ceeb ntawm cov tshuaj tua kab hauv tshuaj yej [4]. Cov hlau hnyav tuaj yeem khaws cia hauv tshuaj yej thiab ua rau muaj tshuaj lom, uas feem ntau yog los ntawm cov av, chiv thiab cua [5-7]. Raws li rau lwm yam kev ua qias tuaj tshwm hauv cov tshuaj yej, nws yog qhov nyuaj heev los txheeb xyuas vim yog cov txheej txheem nyuaj ntawm cov tshuaj yej chains xws li cog, ua, pob, khaws cia thiab kev thauj mus los. PAHs nyob rau hauv tshuaj yej yog los ntawm cov deposition ntawm lub tsheb exhausts thiab combustion ntawm fuels siv thaum lub sij hawm ua cov tshuaj yej nplooj, xws li taws tswm ciab thiab thee [8-10].

Thaum lub sij hawm cov thee thiab hluav taws combustion, cov pa phem xws li carbon oxides yog tsim [11]. Raws li qhov tshwm sim, nws raug cuam tshuam rau cov seem ntawm cov pa phem uas tau hais los saum toj no tshwm sim hauv cov khoom lag luam, xws li cov nplej, cov khoom lag luam haus luam yeeb thiab cov ntses ntses, thaum kub kub, ua rau muaj kev hem thawj rau tib neeg kev noj qab haus huv[12,13]. PAHs tshwm sim los ntawm combustion yog muab los ntawm volatilization ntawm PAHs muaj nyob rau hauv cov fuels nws tus kheej, qhov kub-kub decomposition ntawm aromatic tebchaw thiab cov compound cov tshuaj tiv thaiv ntawm dawb radicals [14]. combustion kub, lub sij hawm, thiab cov ntsiab lus oxygen yog qhov tseem ceeb uas cuam tshuam rau kev hloov pauv ntawm PAHs. Nrog rau qhov nce ntawm qhov kub thiab txias, cov ntsiab lus PAHs thawj zaug tau nce thiab tom qab ntawd txo qis, thiab tus nqi siab tshaj plaws tshwm sim ntawm 800 ° C; Cov ntsiab lus PAHs poob qis heev rau kev taug qab nrog lub sijhawm combustion ntau dua thaum nws qis dua qhov kev txwv hu ua 'hloov lub sijhawm', nrog kev nce ntawm cov pa oxygen hauv huab cua combustion, PAHs emissions txo qis, tab sis tsis tiav oxidation yuav tsim OPAHs thiab lwm yam derivatives [15 —17] ib.

9,10-Anthraquinone (AQ, CAS: 84-65-1, Fig. 1), ib qho oxygen-muaj derivative ntawm PAHs [18], muaj peb lub voj voog condensed. Nws tau teev tseg raws li qhov ua tau carcinogen (Pawg 2B) los ntawm Lub Chaw Haujlwm Saib Xyuas Kev Tshawb Fawb Thoob Ntiaj Teb rau Cancer hauv 2014[19]. AQ tuaj yeem lom rau topoisomerase II cleavage complex thiab inhibit hydrolysis ntawm adenosine triphosphate (ATP) los ntawm DNA topoisomerase II, ua rau DNA ob-strand so, uas txhais tau hais tias ntev ntev raug nyob rau hauv AQ-muaj ib puag ncig thiab ncaj qha kev sib cuag nrog qib siab ntawm AQ. tuaj yeem ua rau DNA puas, kev hloov pauv thiab ua rau muaj kev pheej hmoo mob qog noj ntshav [20]. Raws li kev tsis zoo rau tib neeg kev noj qab haus huv, AQ qhov siab tshaj qhov txwv tsis pub (MRL) ntawm 0.02 mg / kg tau teeb tsa hauv tshuaj yej los ntawm European Union. Raws li peb cov kev tshawb fawb yav dhau los, qhov tso nyiaj ntawm AQ tau pom tias yog qhov tseem ceeb thaum cog tshuaj yej [21]. Tsis tas li ntawd, raws li kev sim ua tshwm sim hauv Indonesian ntsuab thiab dub tshuaj yej ua, nws pom tseeb tias qib AQ hloov pauv loj heev thiab cov pa luam yeeb los ntawm cov khoom siv tau pom zoo tias yog ib qho laj thawj tseem ceeb[22]. Txawm li cas los xij, qhov tseeb keeb kwm ntawm AQ hauv kev tsim tshuaj yej tseem tsis paub, txawm hais tias qee qhov kev xav ntawm AQ tshuaj txoj hauv kev tau pom zoo [23,24], qhia tias nws yog ib qho tseem ceeb heev los txiav txim siab qhov tseem ceeb cuam tshuam rau qib AQ hauv kev ua tshuaj yej.

Daim duab 1. Cov tshuaj formula ntawm AQ.

Muab cov kev tshawb fawb txog kev tsim cov AQ thaum lub sij hawm coal combustion thiab lub peev xwm ntawm fuels nyob rau hauv tshuaj yej processing, ib qho kev sib piv sim tau ua los piav qhia txog cov txiaj ntsig ntawm kev ua cov khoom cua sov ntawm AQ hauv tshuaj yej thiab cua, kev tshuaj xyuas ntau ntawm cov kev hloov ntawm AQ cov ntsiab lus. ntawm cov txheej txheem sib txawv, uas yuav pab tau kom paub meej qhov tseeb keeb kwm, tshwm sim qauv thiab qib ntawm AQ kuab paug hauv tshuaj yej ua.

TSEEM CEEB
Txoj kev validation
Piv nrog rau peb txoj kev tshawb fawb yav dhau los [21], cov txheej txheem ua kua-kua tau muab tso ua ke ua ntej txhaj tshuaj rau GC-MS / MS txhawm rau txhim kho rhiab heev thiab tswj cov lus qhia. Nyob rau hauv daim duab 2b, txoj kev txhim kho pom tau tias muaj kev txhim kho tseem ceeb hauv kev ua kom huv ntawm cov qauv, cov kuab tshuaj los ua xim xim. Nyob rau hauv daim duab 2a, ib tug tag nrho scan spectrum (50-350 m / z) qhia tau hais tias tom qab purification, lub hauv paus kab ntawm MS spectrum txo kom pom tseeb thiab tsawg chromatographic peaks muaj, qhia tau hais tias ib tug loj tus naj npawb ntawm interfering compounds raug tshem tawm tom qab lub kua-kua extraction.

Daim duab 2. (a) Tag nrho scan spectrum ntawm tus qauv ua ntej thiab tom qab kev ua kom huv. (b) Cov nyhuv purification ntawm txoj kev txhim kho.
Txoj kev validation, nrog rau linearity, rov qab, txwv ntawm quantitation (LOQ) thiab matrix nyhuv (ME), yog muaj nyob rau hauv Table 1. Nws yog txaus siab kom tau cov linearity nrog cov coefficient ntawm kev txiav txim siab (r2) siab tshaj 0.998, uas ranged ntawm 0.005. rau 0.2 mg / kg hauv tshuaj yej matrix thiab acetonitrile hnyav, thiab hauv cov qauv huab cua nrog ntau yam ntawm 0.5 txog 8 μg / m3.

Kev rov qab los ntawm AQ raug soj ntsuam ntawm peb qhov sib txawv ntawm qhov ntsuas thiab qhov tseeb hauv cov tshuaj yej qhuav (0.005, 0.02, 0.05 mg / kg), cov tshuaj yej tshiab (0.005, 0.01, 0.02 mg / kg) thiab cov qauv huab cua (0.5, 1.5, 3 μg / m3). Rov qab ntawm AQ hauv tshuaj yej muaj li ntawm 77.78% mus rau 113.02% hauv cov tshuaj yej qhuav thiab los ntawm 96.52% mus rau 125.69% hauv tshuaj yej tua, nrog RSD% qis dua 15%. Rov qab ntawm AQ hauv cov qauv huab cua nyob ntawm 78.47% mus rau 117.06% nrog RSD% qis dua 20%. Qhov qis tshaj qhov siab tshaj plaws tau pom tias yog LOQ, uas yog 0.005 mg / kg, 0.005 mg / kg thiab 0.5 μg / m³ hauv tshuaj yej tua, tshuaj yej qhuav thiab huab cua kuaj, feem. Raws li teev nyob rau hauv Table 1, lub matrix ntawm qhuav tshuaj yej thiab tshuaj yej tua me ntsis nce AQ teb, ua rau ME ntawm 109.0% thiab 110.9%. Raws li rau matrix ntawm cov qauv huab cua, ME yog 196.1%.

Cov theem ntawm AQ thaum lub sijhawm ua tshuaj yej ntsuab
Nrog lub hom phiaj ntawm kev tshawb nrhiav qhov cuam tshuam ntawm qhov sib txawv ntawm cov cua sov ntawm cov tshuaj yej thiab kev ua haujlwm ib puag ncig, ib pawg ntawm cov nplooj tshiab tau muab faib ua ob pawg tshwj xeeb thiab ua tiav cais hauv ob lub chaw ua haujlwm hauv tib lub tuam txhab. Ib pawg tau muab hluav taws xob, thiab lwm pab nrog thee.

Raws li pom nyob rau hauv daim duab 3, AQ theem nrog hluav taws xob raws li qhov cua sov qhov chaw nyob ntawm 0.008 txog 0.013 mg / kg. Thaum lub sij hawm fixation txheej txheem, parching ntawm tshuaj yej nplooj tshwm sim los ntawm kev ua nyob rau hauv lub lauj kaub nrog kub kub ua rau ib tug 9.5% nce nyob rau hauv AQ. Tom qab ntawd, theem ntawm AQ tseem nyob rau hauv cov txheej txheem dov txawm tias tsis muaj kua txiv hmab txiv ntoo, qhia tias cov txheej txheem ntawm lub cev yuav tsis cuam tshuam rau qib AQ hauv kev ua tshuaj yej. Tom qab thawj kauj ruam ziab, AQ qib nce me ntsis ntawm 0.010 mus rau 0.012 mg / kg, tom qab ntawd txuas ntxiv nce mus rau 0.013 mg / kg kom txog thaum kawg ntawm kev rov ziab. PFs, uas qhia tau hais tias qhov sib txawv ntawm txhua kauj ruam, yog 1.10, 1.03, 1.24, 1.08 hauv fixation, dov, thawj ziab thiab rov ziab dua, raws li. Cov txiaj ntsig ntawm PFs qhia tias kev ua haujlwm hauv hluav taws xob muaj qhov cuam tshuam me ntsis ntawm qib AQ hauv tshuaj yej.

Daim duab 3. Qib AQ thaum lub sijhawm ua cov tshuaj yej ntsuab nrog hluav taws xob thiab cov thee ua cov khoom cua sov.
Nyob rau hauv cov ntaub ntawv ntawm thee raws li lub tshav kub qhov chaw, cov ntsiab lus AQ sharply nce thaum lub sij hawm cov tshuaj yej ua, surging los ntawm 0.008 mus rau 0.038 mg / kg. 338.9% AQ tau nce hauv cov txheej txheem kho, mus txog 0.037 mg / kg, uas deb tshaj li MRL ntawm 0.02 mg / kg tau teeb tsa los ntawm European Union. Thaum lub sij hawm dov theem, theem ntawm AQ tseem nce 5.8% txawm tias nyob deb ntawm lub tshuab fixation. Hauv thawj zaug ziab thiab rov ua kom qhuav, AQ cov ntsiab lus tau nce me ntsis lossis txo qis me ntsis. Cov PFs siv cov thee ua qhov cua sov hauv kev kho, dov thawj zaug kom qhuav thiab rov ua kom qhuav yog 4.39, 1.05, 0.93, thiab 1.05, raws li.

Txhawm rau txiav txim siab ntxiv txog kev sib raug zoo ntawm cov thee combustion thiab AQ cov pa phem, cov teeb meem raug tshem tawm (PMs) hauv huab cua hauv kev cob qhia hauv qab ob qhov chaw cua sov tau sau rau kev ntsuas huab cua, raws li qhia hauv daim duab 4. AQ theem ntawm PMs nrog cov thee raws li Qhov kub ntawm qhov hluav taws xob yog 2.98 μg / m3, uas yog ntau tshaj peb zaug siab dua li qhov hluav taws xob 0.91 μg / m3.

Daim duab 4. Cov theem ntawm AQ nyob rau hauv ib puag ncig uas muaj hluav taws xob thiab thee raws li qhov cua sov. * Qhia qhov sib txawv tseem ceeb hauv qib AQ hauv cov qauv (p <0.05).

Cov theem ntawm AQ thaum lub sij hawm oolong tshuaj yej ua Oolong tshuaj yej, feem ntau ua nyob rau hauv Fujian thiab Taiwan, yog ib feem ntawm cov tshuaj yej fermented. Txhawm rau txiav txim siab ntxiv cov kauj ruam tseem ceeb ntawm kev nce qib AQ thiab qhov cuam tshuam ntawm cov roj sib txawv, tib lub batch ntawm cov nplooj tshiab tau ua rau hauv oolong tshuaj yej nrog cov thee thiab cov roj hluav taws xob hybrid raws li qhov chaw tshav kub, ib txhij. Cov qib AQ hauv oolong tshuaj yej ua siv cov khoom siv hluav taws xob sib txawv tau qhia hauv daim duab 5. Rau oolong tshuaj yej ua nrog ntuj gas-hluav taws xob hybrid, qhov sib txawv ntawm qib AQ yog stagnating qis dua 0.005 mg / kg, uas zoo ib yam li cov tshuaj yej ntsuab. nrog hluav taws xob.

Daim duab 5. Qib AQ thaum lub sij hawm oolong tshuaj yej ua nrog ntuj gas-hluav taws xob sib tov thiab thee ua cua sov.

Nrog cov thee ua cov cua sov, cov qib AQ hauv thawj ob kauj ruam, withering thiab ua ntsuab, yog qhov tseem ceeb zoo ib yam li cov roj hluav taws xob sib xyaw. Txawm li cas los xij, cov txheej txheem txuas ntxiv mus txog thaum kho pom qhov sib txawv tau nthuav dav zuj zus, thaum lub sijhawm AQ nce siab ntawm 0.004 txog 0.023 mg / kg. Cov qib hauv cov txheej txheem dov tau txo qis mus rau 0.018 mg / kg, uas tej zaum yuav yog vim qhov poob ntawm cov kua txiv hmab txiv ntoo nqa tawm qee cov kab mob AQ. Tom qab lub dov theem, theem nyob rau hauv qhuav theem tau nce mus rau 0.027 mg / kg. Nyob rau hauv withering, ua ntsuab, fixation, ntim dov thiab ziab, PFs yog 2.81, 1.32, 5.66, 0.78, thiab 1.50, raws li.

Qhov tshwm sim ntawm AQ hauv cov khoom siv tshuaj yej nrog cov khoom siv hluav taws xob sib txawv

Txhawm rau txiav txim siab txog qhov cuam tshuam ntawm AQ cov ntsiab lus ntawm cov tshuaj yej nrog qhov sib txawv ntawm cov cua sov, 40 cov qauv tshuaj yej los ntawm cov kev cob qhia tshuaj yej siv hluav taws xob lossis cov thee raws li cov khoom siv hluav taws xob tau txheeb xyuas, raws li qhia hauv Table 2. Piv nrog rau kev siv hluav taws xob ua hluav taws xob, cov thee muaj ntau tshaj Kev soj ntsuam tus nqi (85.0%) nrog qhov siab tshaj plaws AQ theem ntawm 0.064 mg / kg, qhia tau hais tias nws yooj yim ua rau AQ paug los ntawm fumes uas tsim los ntawm cov thee combustion, thiab tus nqi ntawm 35.0% tau soj ntsuam nyob rau hauv cov qauv ntawm cov thee. Feem ntau conspicuously, hluav taws xob muaj qhov tsawg tshaj plaws detective thiab excedance tus nqi ntawm 56.4% thiab 7.7% feem, nrog rau cov ntsiab lus siab tshaj plaws ntawm 0.020 mg / kg.

Kev sib tham

Raws li PFs thaum ua haujlwm nrog ob hom kev siv hluav taws xob, nws tau pom tseeb tias kev kho yog lub hauv paus tseem ceeb uas ua rau nce qib AQ hauv tshuaj yej ntau lawm nrog cov thee thiab kev ua haujlwm hauv hluav taws xob muaj qhov cuam tshuam me ntsis ntawm cov ntsiab lus ntawm AQ. hauv tshuaj yej. Thaum lub sij hawm ua cov tshuaj yej ntsuab, thee combustion ua ib tug ntau ntawm fumes nyob rau hauv lub fixation txheej txheem piv nrog rau cov hluav taws xob cua sov txheej txheem, qhia tau hais tias tej zaum fumes yog lub ntsiab ntawm AQ kua paug los ntawm kev sib cuag nrog tshuaj yej tua instantly hauv tshuaj yej ua, zoo ib yam li cov txheej txheem raug nyob rau hauv cov qauv ntawm cov pa luam yeeb [25]. Qhov nce me ntsis ntawm AQ cov ntsiab lus thaum lub sij hawm dov theem qhia tias cov pa taws tshwm sim los ntawm cov thee combustion tsis tsuas cuam tshuam rau qib AQ thaum lub sij hawm kho, tab sis kuj nyob rau hauv qhov chaw ua hauj lwm vim atmospheric deposition. Coals kuj tau siv los ua qhov cua sov hauv thawj zaug ziab thiab rov ua kom qhuav, tab sis nyob rau hauv ob kauj ruam no cov ntsiab lus AQ nce me ntsis los yog txo qis me ntsis. Qhov no tuaj yeem piav qhia los ntawm qhov tseeb tias lub tshuab ziab khaub ncaws kub kub tau khaws cov tshuaj yej kom deb ntawm cov pa taws los ntawm cov thee combustion[26]. Txhawm rau txiav txim siab qhov muaj kuab paug, cov qib AQ hauv huab cua tau txheeb xyuas, ua rau muaj qhov sib txawv tseem ceeb ntawm ob lub rooj cob qhia. Qhov laj thawj tseem ceeb rau qhov no yog tias cov thee siv hauv kev kho, thawj zaug ziab thiab rov ua kom qhuav yuav ua rau AQ thaum tsis tiav combustion. Cov AQ no ces adsorbed nyob rau hauv cov me me ntawm cov khib nyiab tom qab coal combustion thiab dispersed nyob rau hauv cov huab cua, elevating cov theem ntawm AQ pa phem nyob rau hauv lub rhiav ib puag ncig [15]. Sij hawm dhau mus, vim qhov loj ntawm thaj chaw tshwj xeeb thiab lub peev xwm adsorption ntawm cov tshuaj yej, cov khoom no tau nyob rau saum npoo ntawm cov tshuaj yej nplooj, uas ua rau nce ntawm AQ hauv kev tsim khoom. Yog li ntawd, thee combustion tau xav tias yog txoj hauv kev tseem ceeb uas ua rau muaj AQ ntau dhau ntawm kev ua tshuaj yej, nrog cov pa taws ua rau muaj kuab paug.

Raws li rau oolong tshuaj yej ua, AQ tau nce nyob rau hauv kev ua nrog ob qhov chaw tshav kub, tab sis qhov sib txawv ntawm ob qhov chaw tshav kub yog qhov tseem ceeb. Cov txiaj ntsig kuj tau qhia tias cov thee ua qhov cua sov ua lub luag haujlwm tseem ceeb hauv kev nce qib AQ, thiab kev txhim kho tau suav tias yog kauj ruam tseem ceeb rau kev ua kom muaj kab mob AQ hauv oolong tshuaj yej ua raws li PFs. Thaum lub sij hawm oolong tshuaj yej ua nrog natural gas-hluav taws xob hybrid raws li ib tug tshav kub qhov chaw, tus qauv ntawm AQ theem yog stagnating hauv qab no 0.005 mg / kg, uas zoo ib yam li cov tshuaj yej ntsuab nrog hluav taws xob, qhia tias lub zog huv si, xws li hluav taws xob thiab ntuj. roj, tuaj yeem txo qhov kev pheej hmoo ntawm kev tsim cov kab mob AQ los ntawm kev ua haujlwm.

Raws li kev kuaj ntsuas, cov txiaj ntsig tau pom tias qhov xwm txheej ntawm AQ paug tsis zoo yog qhov phem dua thaum siv cov thee los ua qhov cua sov ntau dua li hluav taws xob, uas tuaj yeem yog vim cov pa taws los ntawm kev sib tsoo ntawm cov thee los rau hauv cov tshuaj yej nplooj thiab nyob ib ncig ntawm qhov chaw ua haujlwm. Txawm li cas los xij, txawm hais tias nws tau pom tseeb tias hluav taws xob yog qhov chaw sov tshaj plaws thaum lub sijhawm ua tshuaj yej, tseem muaj cov kab mob AQ hauv cov tshuaj yej cov khoom siv hluav taws xob los ua qhov cua sov. Qhov xwm txheej zoo li me ntsis zoo ib yam li yav dhau los ua haujlwm uas cov tshuaj tiv thaiv ntawm 2- alkenals nrog hydroquinones thiab benzoquinones tau pom tias yog txoj hauv kev muaj peev xwm tshuaj lom neeg [23], vim li cas rau qhov no yuav raug tshawb xyuas hauv kev tshawb fawb yav tom ntej.

Cov lus xaus

Hauv kev ua haujlwm no, qhov muaj peev xwm ntawm AQ cov pa phem hauv cov tshuaj yej ntsuab thiab oolong tau lees paub los ntawm kev sim sib piv raws li kev txhim kho GC-MS / MS analytical method. Peb qhov kev tshawb pom ncaj qha tau txhawb nqa tias cov pa phem tseem ceeb ntawm cov qib siab ntawm AQ yog fume tshwm sim los ntawm combustion, uas tsis tsuas yog cuam tshuam rau theem ua tab sis kuj cuam tshuam rau qhov chaw ua haujlwm. Tsis zoo li nyob rau hauv cov dov thiab withering theem, qhov twg cov kev hloov nyob rau hauv lub theem ntawm AQ yog inconspicuous, cov theem nrog ncaj qha kev koom tes ntawm cov thee thiab taws, xws li fixation, yog lub ntsiab txheej txheem nyob rau hauv uas AQ paug tau sawv vim tus nqi ntawm kev sib cuag ntawm cov tshuaj yej. thiab fumes thaum lub sij hawm no. Yog li ntawd, cov roj huv huv xws li cov pa roj ntsha thiab hluav taws xob tau pom zoo ua cov cua kub hauv kev ua tshuaj yej. Tsis tas li ntawd, cov txiaj ntsig kev sim kuj tau pom tias thaum tsis muaj cov pa taws uas tsim los ntawm kev sib xyaw, tseem muaj lwm yam ua rau trace AQ thaum lub sijhawm ua tshuaj yej, thaum me me ntawm AQ kuj tau pom nyob rau hauv kev cob qhia nrog cov roj huv, uas yuav tsum tau tshawb xyuas ntxiv. hauv kev tshawb fawb yav tom ntej.

Cov khoom siv thiab cov txheej txheem

Reagents, tshuaj thiab khoom siv

Anthraquinone tus qauv (99.0%) tau yuav los ntawm Dr. Ehrenstorfer GmbH Company (Augsburg, Lub teb chaws Yelemees). D8-Anthraquinone tus qauv sab hauv (98.6%) tau yuav los ntawm C / D / N Isotopes (Quebec, Canada). Anhydrous sodium sulfate (Na2SO4) thiab magnesium sulfate (MgSO4) (Shanghai, Suav). Florisil tau muab los ntawm Wenzhou Organic Chemical Company (Wenzhou, Suav). Daim iav iav fiber ntau (90 hli) tau yuav los ntawm Ahlstrom-munksjö tuam txhab (Helsinki, Finland).

Kev npaj ua qauv

Cov qauv tshuaj yej ntsuab tau ua tiav nrog kev txhim kho, dov, thawj zaug ziab thiab rov ua kom qhuav (siv cov khoom siv kaw), thaum cov tshuaj yej oolong tshuaj yej tau ua tiav nrog withering, ua ntsuab (pob zeb thiab sawv cov nplooj tshiab hloov), kho, ntim dov, thiab ziab. Cov qauv ntawm txhua kauj ruam tau sau peb zaug ntawm 100g tom qab sib xyaw kom zoo. Tag nrho cov qauv tau muab khaws cia ntawm -20 ° C rau kev soj ntsuam ntxiv.

Cov qauv huab cua tau sau los ntawm iav fiber ntau daim ntawv (90 hli) siv nruab nrab ntim samplers (PTS-100, Qingdao Laoshan Electronic Instrument Company, Qingdao, Suav teb) [27], khiav ntawm 100 L / min rau 4 h.

Fortified kuaj tau spiked nrog AQ ntawm 0.005 mg / kg, 0.010 mg / kg, 0.020 mg / kg rau cov tshuaj yej tshiab, ntawm 0.005 mg / kg, 0.020 mg / kg, 0.050 mg / kg rau qhuav tshuaj yej thiab ntawm 0.012 mg / kg. (0.5 µg / m3 rau cov qauv huab cua), 0.036 mg / kg (1.5 µg / m3 rau huab cua smaple), 0.072 mg / kg (3.0 µg / m3 rau cov qauv huab cua) rau iav lim ntawv, feem. Tom qab co kom huv si, tag nrho cov qauv raug tso tseg rau 12 teev, ua raws li kev rho tawm thiab ntxuav cov kauj ruam.

Cov ntsiab lus noo noo tau txais los ntawm kev noj 20 g ntawm cov qauv tom qab sib tov txhua kauj ruam, cua sov ntawm 105 ° C rau 1 h, tom qab ntawd hnyav thiab rov ua dua peb zaug thiab coj tus nqi nruab nrab thiab muab faib los ntawm qhov hnyav ua ntej cua sov.

Sample extraction thiab ntxuav

Tshuaj yej qauv: Kev rho tawm thiab ua kom huv ntawm AQ los ntawm cov tshuaj yej cov qauv tau ua raws li cov qauv luam tawm los ntawm Wang li al. nrog ntau yam kev hloov pauv [21]. Luv luv, 1.5 g ntawm tshuaj yej cov qauv yog thawj zaug tov nrog 30 μL D8-AQ (2 mg / kg) thiab sab laug rau sawv ntsug rau 30 feeb, ces zoo tov nrog 1.5 mL deionized dej thiab sab laug rau sawv ntsug rau 30 feeb. 15 mL 20% acetone hauv n-hexane tau ntxiv rau cov tshuaj yej kuaj thiab sonicated rau 15 min. Tom qab ntawd cov qauv tau vortexed nrog 1.0 g MgSO4 rau 30 s, thiab centrifuged rau 5 min, ntawm 11,000 rpm. Tom qab tau tsiv mus rau 100 mL pear-puab flasks, 10 mL ntawm cov organic theem tau evaporated mus rau yuav luag qhuav nyob rau hauv lub tshuab nqus tsev ntawm 37 ° C. 5 mL 2.5% acetone nyob rau hauv n-hexane re-solved cov extract nyob rau hauv pear-zoo li lub hwj rau purification. Cov iav kem (10 cm × 0.8 cm) muaj nyob hauv qab mus rau sab saum toj ntawm iav ntaub plaub thiab 2g florisil, uas nyob nruab nrab ntawm ob txheej ntawm 2 cm Na2SO4. Tom qab ntawd 5 mL ntawm 2.5% acetone hauv n-hexane prewashed kem. Tom qab thauj cov tshuaj redissolved, AQ tau eluted peb zaug nrog 5 mL, 10 mL, 10 mL ntawm 2.5% acetone hauv n-hexane. Cov eluates sib xyaw ua ke tau hloov mus rau pear-shaped flasks thiab evaporated rau yuav luag qhuav nyob rau hauv lub tshuab nqus tsev ntawm 37 ° C. Tom qab ntawd cov khoom seem qhuav tau rov ua dua nrog 1 mL ntawm 2.5% acetone hauv hexane ua raws li kev pom los ntawm 0.22 µm pore loj lim. Tom qab ntawd cov tshuaj reconstituted yog tov nrog acetonitrile ntawm lub ntim piv ntawm 1: 1. Tom qab tuav cov kauj ruam, tus subnatant tau siv rau GC-MS / MS tsom xam.

Cov qauv huab cua: Ib nrab ntawm cov ntawv fiber ntau, dripped nrog 18 μL d8-AQ (2 mg / kg), yog immersed nyob rau hauv 15 mL ntawm 20% acetone hauv n-hexane, ces sonicated rau 15 min. Cov theem organic tau sib cais los ntawm centrifugation ntawm 11,000 rpm rau 5 min thiab tag nrho cov txheej sab saud raug muab tshem tawm hauv lub khob pear. Tag nrho cov theem ntawm cov organic yog evaporated mus rau yuav luag qhuav nyob rau hauv lub tshuab nqus tsev ntawm 37 ° C. 5 mL ntawm 2.5% acetone hauv hexane redissolved cov extracts rau purification tib yam li hauv cov tshuaj yej kuaj.

GC-MS/MS tsom xam

Varian 450 roj chromatograph nruab nrog Varian 300 tandem huab cua ntes (Varian, Walnut Creek, CA, USA) tau siv los ua AQ tsom xam nrog MS WorkStation version 6.9.3 software. Varian Factor Four capillary kem VF-5ms (30 m × 0.25 mm × 0.25 μm) tau siv rau kev sib cais chromatographic. Cov pa roj carbon monoxide, helium (> 99.999%), tau teeb tsa tus nqi tas li ntawm 1.0 mL / min nrog cov roj sib tsoo ntawm Argon (> 99.999%). Qhov cub kub pib los ntawm 80 ° C thiab tuav rau 1 min; nce ntawm 15 ° C / min mus rau 240 ° C, ces mus txog 260 ° C ntawm 20 ° C / min thiab tuav rau 5 feeb. Qhov kub ntawm qhov chaw ion yog 210 ° C, nrog rau kev hloov kab kub ntawm 280 ° C. Kev txhaj tshuaj yog 1.0 μL. Cov xwm txheej MRM tau qhia hauv Table 3.

Agilent 8890 gas chromatograph nruab nrog Agilent 7000D triple quadrupole mass spectrometer (Agilent, Stevens Creek, CA, USA) tau siv los tshuaj xyuas cov nyhuv purification nrog MassHunter version 10.1 software. Agilent J&W HP-5ms GC Kem (30 m × 0.25 mm × 0.25 μm) tau siv rau kev sib cais chromatographic. Cov pa roj carbon monoxide, Helium (> 99.999%), tau teeb tsa ntawm tus nqi ntws tsis tu ncua ntawm 2.25 mL / min nrog cov roj sib tsoo ntawm Nitrogen (> 99.999%). Qhov kub ntawm EI ion qhov chaw tau hloov kho ntawm 280 ° C, tib yam li cov kab hloov pauv kub. Qhov cub kub pib los ntawm 80 ° C thiab tuav rau 5 min; tsa los ntawm 15 ° C / min mus rau 240 ° C, ces mus txog 280 ° C ntawm 25 ° C / min thiab khaws cia rau 5 min. Cov xwm txheej MRM tau qhia hauv Table 3.

Kev txheeb cais
Cov ntsiab lus AQ hauv cov nplooj tshiab tau raug kho kom qhuav cov ntsiab lus los ntawm kev faib los ntawm cov ntsiab lus noo noo txhawm rau sib piv thiab txheeb xyuas qib AQ thaum ua.

Cov kev hloov pauv ntawm AQ hauv cov qauv tshuaj yej tau soj ntsuam nrog Microsoft Excel software thiab IBM SPSS Statistics 20.

Cov txheej txheem ua haujlwm tau siv los piav qhia txog cov kev hloov pauv hauv AQ thaum lub sijhawm ua tshuaj yej. PF = Rl / Rf , qhov twg Rf yog qib AQ ua ntej ua cov kauj ruam thiab Rl yog qib AQ tom qab ua cov kauj ruam. PF qhia txog qhov txo qis (PF <1) lossis nce (PF> 1) hauv AQ residual thaum lub sijhawm ua haujlwm tshwj xeeb.

ME qhia txog qhov txo qis (ME <1) lossis nce (ME> 1) hauv cov lus teb rau cov cuab yeej tshuaj ntsuam xyuas, uas yog raws li qhov piv ntawm cov nqes hav ntawm calibration hauv matrix thiab hnyav raws li hauv qab no:

ME = (slopematrix/slopesolvent − 1) × 100%

Qhov twg slopematrix yog txoj kab nqes ntawm calibration nkhaus hauv matrix-matched hnyav, slopesolvent yog txoj kab nqes ntawm calibration nkhaus hauv hnyav.

TXOJ CAI
Txoj haujlwm no tau txais kev txhawb nqa los ntawm Science thiab Technology Major Project hauv Zhejiang Province (2015C12001) thiab National Science Foundation of China (42007354).
Kev tsis sib haum xeeb
Cov kws sau ntawv tshaj tawm tias lawv tsis muaj kev cuam tshuam ntawm kev txaus siab.
Txoj cai thiab kev tso cai
Copyright: © 2022 los ntawm tus sau. Exclusive Licensee Maximum Academic Press, Fayetteville, GA. Kab lus no yog ib tsab xov xwm qhib tau muab faib raws li Creative Commons Attribution License (CC BY 4.0), mus saib https://creativecommons.org/licenses/by/4.0/.
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Hais txog tsab xov xwm no
Sau tsab xov xwm no
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