Ndemanga
9,10-Anthraquinone (AQ) ndi chodetsa chomwe chili ndi chiopsezo choyambitsa khansa ndipo chimapezeka mu tiyi padziko lonse lapansi. Kuchuluka kotsalira (MRL) kwa AQ mu tiyi yokhazikitsidwa ndi European Union (EU) ndi 0.02 mg/kg. Zomwe zingatheke za AQ pokonza tiyi ndi magawo akuluakulu a zochitika zake zidafufuzidwa potengera njira yosinthira ya AQ ndi kusanthula kwa gas chromatography-tandem mass spectrometry (GC-MS/MS). Poyerekeza ndi magetsi monga gwero la kutentha pakupanga tiyi wobiriwira, AQ idakwera ndi 4.3 mpaka 23.9 pakukonza tiyi ndi malasha ngati gwero la kutentha, kupitilira 0.02 mg/kg, pomwe mulingo wa AQ m'chilengedwe unachulukitsa katatu. Zomwezo zidawonedwanso pokonza tiyi wa oolong pansi pa kutentha kwa malasha. Masitepe okhudzana mwachindunji pakati pa masamba a tiyi ndi utsi, monga kukonza ndi kuyanika, amatengedwa ngati njira zazikulu zopangira AQ pokonza tiyi. Miyezo ya AQ idakula ndi kukwera kwa nthawi yolumikizana, kutanthauza kuti kuchuluka kwa AQ woyipitsidwa mu tiyi kumatha kuchoka ku utsi wobwera chifukwa cha malasha ndi kuyaka. Zitsanzo makumi anayi kuchokera ku zokambirana zosiyana ndi magetsi kapena malasha monga magwero a kutentha adawunikidwa, kuchokera ku 50.0% -85.0% ndi 5.0% -35.0% kuti azindikire ndi kupitirira mitengo ya AQ. Kuphatikiza apo, kuchuluka kwa AQ kwa 0.064 mg/kg kudawonedwa mu tiyi yokhala ndi malasha ngati gwero la kutentha, zomwe zikuwonetsa kuti kuipitsidwa kwakukulu kwa AQ muzinthu za tiyi kumatha kuthandizidwa ndi malasha.
Keywords: 9,10-Anthraquinone, Kukonza tiyi, Malasha, Gwero loyipitsidwa
MAU OYAMBA
Tiyi wopangidwa kuchokera ku masamba a chitsamba chobiriwira cha Camellia sinensis (L.) O. Kuntze, ndi chakumwa chodziwika bwino padziko lonse lapansi chifukwa cha kukoma kwake kotsitsimula komanso thanzi. Mu 2020 padziko lonse lapansi, kupanga tiyi kudakwera mpaka matani 5,972 miliyoni, zomwe zidakwera kawiri pazaka 20 zapitazi[1]. Kutengera njira zosiyanasiyana zopangira, pali mitundu isanu ndi umodzi ya tiyi, kuphatikiza tiyi wobiriwira, tiyi wakuda, tiyi wakuda, tiyi wa oolong, tiyi woyera ndi tiyi wachikasu[2,3]. Kuonetsetsa kuti zinthu zili bwino komanso zotetezeka, ndikofunikira kuyang'anira kuchuluka kwa zoipitsa ndikutanthauzira komwe zidachokera.

Kuzindikiritsa magwero a zowononga, monga zotsalira za mankhwala, zitsulo zolemera ndi zowononga zina monga polycyclic aromatic hydrocarbons (PAHs), ndiye sitepe yoyamba yoletsa kuipitsa. Kupopera mankhwala mwachindunji m'minda ya tiyi, komanso kutengeka kwa mpweya chifukwa cha ntchito pafupi ndi minda ya tiyi, ndiye gwero lalikulu la zotsalira za mankhwala mu tiyi[4]. Zitsulo zolemera zimatha kuwunjikana mu tiyi ndikupangitsa kuti pakhale poizoni, zomwe zimachokera ku dothi, feteleza ndi mpweya[5-7]. Ponena za kuipitsidwa kwina komwe kumawoneka mosayembekezereka mu tiyi, zinali zovuta kuzizindikira chifukwa cha zovuta za njira zopangira tiyi kuphatikiza minda, kukonza, phukusi, kusungirako ndi mayendedwe. Ma PAH mu tiyi adachokera pakuyika utsi wagalimoto komanso kuyaka kwamafuta omwe amagwiritsidwa ntchito pokonza masamba a tiyi, monga nkhuni ndi malasha[8-10].

Pa kuyaka kwa malasha ndi nkhuni, zowononga monga ma carbon oxides amapangidwa[11]. Chotsatira chake, zimakhala zosavuta kuti zotsalira za zowonongeka zomwe zatchulidwazi zichitike muzinthu zowonongeka, monga tirigu, fodya wosuta ndi nsomba zamphaka, pa kutentha kwakukulu, zomwe zikuwopseza thanzi laumunthu [12,13]. Ma PAH omwe amayamba chifukwa cha kuyaka amachokera ku kusinthasintha kwa ma PAH omwe ali mumafuta omwewo, kutentha kwakukulu kwa mankhwala onunkhira komanso momwe zimakhalira pakati pa ma radicals aulere [14]. Kutentha kwa kuyaka, nthawi, ndi okosijeni ndizofunikira zomwe zimakhudza kutembenuka kwa PAHs. Ndi kuwonjezeka kwa kutentha, zinthu za PAH zinayamba kuwonjezeka kenako ndikuchepa, ndipo mtengo wapamwamba unachitika pa 800 ° C; Zomwe zili mu PAHs zinachepa kwambiri kuti zitsatire ndi nthawi yoyaka moto pamene inali pansi pa malire otchedwa 'nthawi yamalire', ndi kuwonjezeka kwa mpweya wa okosijeni mu mpweya woyaka, mpweya wa PAH unachepetsedwa kwambiri, koma okosijeni osakwanira kungapangitse OPAHs ndi zina zotumphukira [15] −17].

9,10-Anthraquinone (AQ, CAS: 84-65-1, Chithunzi 1), chochokera ku PAHs chokhala ndi okosijeni [18], chimakhala ndi maulendo atatu ozungulira. Zinalembedwa ngati zotheka carcinogen (Gulu 2B) ndi International Agency for Research on Cancer mu 2014[19]. AQ imatha kupha topoisomerase II cleavage complex ndikuletsa hydrolysis ya adenosine triphosphate (ATP) ndi DNA topoisomerase II, kupangitsa DNA kusweka kwa chingwe chawiri, zomwe zikutanthauza kuti kuwonekera kwanthawi yayitali pansi pa chilengedwe chokhala ndi AQ ndikulumikizana mwachindunji ndi kuchuluka kwa AQ. kungayambitse kuwonongeka kwa DNA, kusinthika ndi kuonjezera chiopsezo cha khansa[20]. Monga zotsatira zoyipa pa thanzi la munthu, AQ maximum residue limit (MRL) ya 0.02 mg/kg idayikidwa mu tiyi ndi European Union. Malinga ndi maphunziro athu am'mbuyomu, ma depositi a AQ adanenedwa ngati gwero lalikulu pakulima tiyi[21]. Komanso, kutengera zotsatira zoyeserera pakukonza tiyi wobiriwira ndi wakuda waku Indonesia, zikuwonekeratu kuti mulingo wa AQ udasintha kwambiri ndipo utsi wochokera ku zida zopangira zidanenedwa ngati chimodzi mwazifukwa zazikulu[22]. Komabe, chiyambi cholondola cha AQ pakukonza tiyi sichinachitikebe, ngakhale malingaliro ena a njira ya mankhwala a AQ adanenedwa [23,24], kusonyeza kuti ndikofunikira kwambiri kudziwa zinthu zofunika kwambiri zomwe zimakhudza gawo la AQ pakukonza tiyi.

Chithunzi 1. Mankhwala a AQ.

Chifukwa cha kafukufuku wokhudza mapangidwe a AQ pa kuyaka kwa malasha komanso kuopsa kwa mafuta pakupanga tiyi, kuyesa kofananira kunachitika kuti afotokoze zotsatira za kutentha kwa AQ mu tiyi ndi mpweya, kusanthula kachulukidwe ka kusintha kwa zomwe zili mu AQ. pamasitepe osiyanasiyana opangira, zomwe zimathandiza kutsimikizira komwe kumachokera, mawonekedwe ochitika komanso kuchuluka kwa kuipitsidwa kwa AQ pakukonza tiyi.

ZOTSATIRA
Njira yotsimikizira
Poyerekeza ndi phunziro lathu lapitalo [21], njira yochotsera madzi amadzimadzi inaphatikizidwa isanayambe jekeseni ku GC-MS/MS kuti apititse patsogolo kukhudzika ndi kusunga mawu othandiza. Mu Mkuyu 2b, njira yowongoka idawonetsa kusintha kwakukulu pakuyeretsedwa kwachitsanzo, chosungunulira chinakhala chopepuka mumtundu. Mu chithunzi cha 2a, chithunzithunzi chokwanira (50-350 m / z) chikuwonetseratu kuti pambuyo pa kuyeretsedwa, mzere woyambira wa MS spectrum unachepetsedwa mwachiwonekere ndipo nsonga zochepa za chromatographic zinalipo, kusonyeza kuti chiwerengero chachikulu cha mankhwala osokoneza bongo chinachotsedwa pambuyo m'zigawo zamadzimadzi-zamadzimadzi.

Chithunzi 2. (a) Chiwonetsero chokwanira cha sampuli isanayambe komanso itatha kuyeretsedwa. (b) Kuyeretsa kwa njira yabwinoko.
Kutsimikizira njira, kuphatikizapo mzere, kuchira, malire a kuchuluka (LOQ) ndi matrix effect (ME), akuwonetsedwa mu Table 1. Ndizokhutiritsa kupeza mzere ndi coefficient of determination (r2) kuposa 0.998, yomwe inachokera ku 0.005 mpaka 0.2 mg/kg mu tiyi masanjidwewo ndi acetonitrile zosungunulira, ndi mu mpweya zitsanzo ndi osiyanasiyana 0.5 mpaka 8 μg/m3.

Kubwezeretsedwa kwa AQ kunayesedwa pamiyeso itatu ya spiked pakati pa miyeso yoyezera komanso yokhazikika mu tiyi wowuma (0.005, 0.02, 0.05 mg/kg), tiyi watsopano (0.005, 0.01, 0.02 mg/kg) ndi zitsanzo za mpweya (0.5, 1.5, 3) μg/m3). Kuchira kwa AQ mu tiyi kunachokera ku 77.78% mpaka 113.02% mu tiyi wowuma komanso kuchokera 96.52% mpaka 125.69% mu mphukira za tiyi, ndi RSD% yotsika kuposa 15%. Kubwezeretsanso kwa AQ mu zitsanzo za mpweya kunachokera ku 78.47% mpaka 117.06% ndi RSD% pansi pa 20%. Zotsika kwambiri za spiked zidadziwika kuti LOQ, zomwe zinali 0.005 mg/kg, 0.005 mg/kg ndi 0.5 μg/m³ mu mphukira za tiyi, tiyi wouma ndi zitsanzo za mpweya, motsatana. Monga tafotokozera mu Gulu 1, matrix a tiyi wowuma ndi tiyi wowuma adawonjezera pang'ono kuyankha kwa AQ, zomwe zidapangitsa ME ya 109.0% ndi 110.9%. Ponena za masanjidwe a zitsanzo za mpweya, ME inali 196.1%.

Miyezo ya AQ panthawi yopanga tiyi wobiriwira
Ndi cholinga chofuna kudziwa zotsatira za kutentha kosiyanasiyana pa tiyi ndi malo opangira zinthu, masamba atsopano adagawidwa m'magulu awiri ndipo amakonzedwa mosiyana muzochita ziwiri zogwirira ntchito mu bizinesi yomweyo. Gulu lina linaperekedwa ndi magetsi, ndipo lina ndi malasha.

Monga momwe tawonetsera mkuyu 3, mlingo wa AQ ndi magetsi monga gwero la kutentha limachokera ku 0.008 mpaka 0.013 mg / kg. Panthawi yokonza, kuyanika kwa masamba a tiyi chifukwa cha kukonzedwa mumphika wokhala ndi kutentha kwakukulu kunapangitsa kuti AQ ichuluke ndi 9.5%. Kenako, mulingo wa AQ udatsalira panthawi yogubuduza ngakhale madzi atayika, kutanthauza kuti machitidwe amthupi sangakhudze kuchuluka kwa AQ pakukonza tiyi. Pambuyo pa masitepe oyambirira owumitsa, mlingo wa AQ unakula pang'ono kuchokera ku 0.010 mpaka 0.012 mg / kg, kenako unapitirira kukwera mpaka 0.013 mg / kg mpaka kumapeto kwa kuyanikanso. PFs, zomwe zimasonyeza kwambiri kusiyana kwa sitepe iliyonse, zinali 1.10, 1.03, 1.24, 1.08 mu fixation, rolling, first kuyanika ndi kuyanikanso, motero. Zotsatira za PFs zikuwonetsa kuti kukonza pansi pa mphamvu yamagetsi kunakhudza pang'ono kuchuluka kwa AQ mu tiyi.

Chithunzi 3. Mlingo wa AQ panthawi yopanga tiyi wobiriwira ndi magetsi ndi malasha monga magwero a kutentha.
Pankhani ya malasha ngati gwero la kutentha, zomwe zili mu AQ zidakwera kwambiri pakukonza tiyi, kuchokera pa 0.008 mpaka 0.038 mg/kg. 338.9% AQ inawonjezeka mu ndondomeko yokonzekera, kufika pa 0.037 mg / kg, yomwe inadutsa kwambiri MRL ya 0.02 mg / kg yokhazikitsidwa ndi European Union. Panthawi yogubuduza, mulingo wa AQ udakwerabe ndi 5.8% ngakhale anali kutali ndi makina okonzera. Poyanika koyamba ndikuwumitsanso, zomwe zili mu AQ zidakwera pang'ono kapena kuchepa pang'ono. Ma PF omwe amagwiritsa ntchito malasha ngati gwero la kutentha pakukonza, kuyanika koyamba ndi kuyanikanso kunali 4.39, 1.05, 0.93, ndi 1.05, motsatana.

Kuti mudziwenso kugwirizana pakati pa kuyaka kwa malasha ndi kuipitsidwa kwa AQ, nkhani zoyimitsidwa (PMs) mumlengalenga mu zokambirana pansi pa magwero onse a kutentha zinasonkhanitsidwa kuti ziwunikire mpweya, monga momwe tawonetsera pa Chithunzi 4. Mlingo wa AQ wa PMs ndi malasha monga gwero la kutentha linali 2.98 μg/m3, lomwe linali loposa katatu kuposa lomwe linali ndi magetsi 0.91 μg/m3.

Chithunzi 4. Miyezo ya AQ mu chilengedwe ndi magetsi ndi malasha monga gwero la kutentha. * Imawonetsa kusiyana kwakukulu m'magawo a AQ mu zitsanzo (p <0.05).

Miyezo ya AQ pakupanga tiyi wa oolong tiyi wa Oolong, wopangidwa makamaka ku Fujian ndi Taiwan, ndi mtundu wa tiyi wothira pang'ono. Kuti mudziwenso njira zazikulu zowonjezera mulingo wa AQ ndi zotsatira zamafuta osiyanasiyana, masamba omwewo adapangidwa kukhala tiyi wa oolong wokhala ndi malasha ndi gasi-magetsi osakanizidwa ngati magwero otentha, nthawi imodzi. Miyezo ya AQ pakupanga tiyi wa oolong pogwiritsa ntchito magwero osiyanasiyana otentha akuwonetsedwa mkuyu. ndi magetsi.

Chithunzi 5. Mulingo wa AQ pakukonza tiyi wa oolong ndi kuphatikizika kwamagetsi kwa gasi-magetsi ndi malasha ngati gwero la kutentha.

Ndi malasha monga gwero la kutentha, milingo ya AQ m'masitepe awiri oyamba, kufota ndikupanga zobiriwira, zinali zofanana ndi kuphatikiza kwamagetsi achilengedwe a gasi. Komabe, njira zotsatila mpaka kukonzanso kunawonetsa kuti kusiyana kunakula pang'onopang'ono, pomwe mlingo wa AQ unakwera kuchokera ku 0.004 mpaka 0.023 mg / kg. Mulingo wapang'onopang'ono watsika mpaka 0.018 mg/kg, zomwe zitha kukhala chifukwa cha kutayika kwa madzi a tiyi komwe kumatengera zina za AQ. Pambuyo pa kugubuduza siteji, mlingo mu kuyanika siteji unawonjezeka kufika 0.027 mg/kg. Pakufota, kupanga zobiriwira, kukonza, zodzaza ndi kuyanika, ma PF anali 2.81, 1.32, 5.66, 0.78, ndi 1.50, motsatana.

Kupezeka kwa AQ muzinthu za tiyi zokhala ndi kutentha kosiyanasiyana

Kuti mudziwe zotsatira za AQ zomwe zili mu tiyi ndi magwero osiyanasiyana otentha, zitsanzo za tiyi za 40 kuchokera ku zokambirana za tiyi pogwiritsa ntchito magetsi kapena malasha monga magwero a kutentha zinayesedwa, monga momwe tawonetsera mu Table 2. Poyerekeza ndi kugwiritsa ntchito magetsi monga gwero la kutentha, malasha anali ndi mphamvu zambiri. kuchuluka kwa ofufuza (85.0%) ndi kuchuluka kwa AQ kwa 0.064 mg/kg, zomwe zikuwonetsa kuti zinali zosavuta kuyambitsa kuipitsidwa kwa AQ ndi utsi wopangidwa ndi kuyaka kwa malasha, ndipo kuchuluka kwa 35.0% kudawonedwa mu zitsanzo zamakala. Chochititsa chidwi kwambiri, magetsi anali ndi chiwerengero chochepa kwambiri cha ofufuza komanso ochulukirapo a 56.4% ndi 7.7% motsatira, ndi chiwerengero chachikulu cha 0.020 mg / kg.

KAMBIRANANI

Kutengera ma PF panthawi yokonza ndi mitundu iwiri ya magwero otentha, zinali zoonekeratu kuti kukonza ndiye gawo lalikulu lomwe lidapangitsa kuti ma AQ achuluke pakupanga tiyi ndi malasha ndikuwongolera pansi pa mphamvu yamagetsi kudakhudza pang'ono zomwe zili mu AQ. mu tiyi. Panthawi yokonza tiyi wobiriwira, kuyaka kwa malasha kumatulutsa utsi wambiri pokonza tiyi poyerekeza ndi kutenthetsa kwamagetsi, kusonyeza kuti mwina utsi ndiwo udayambitsa zowononga za AQ kuchokera pakukhudzana ndi mphukira za tiyi nthawi yomweyo pokonza tiyi, zomwe zimafanana ndi momwe zimakhalira mu zitsanzo za barbecue wosuta [25]. Kuwonjezeka pang'ono kwa zinthu za AQ panthawi yogubuduza kunasonyeza kuti utsi woyaka chifukwa cha kuyaka kwa malasha sumangokhudza mlingo wa AQ panthawi yokonzekera, komanso m'malo opangira zinthu chifukwa cha mlengalenga. Makala ankagwiritsidwanso ntchito ngati gwero la kutentha poyamba kuyanika ndi kuyanikanso, koma mu masitepe awiriwa zomwe zili mu AQ zinawonjezeka pang'ono kapena kuchepa pang'ono. Izi zitha kufotokozedwa ndi mfundo yakuti chowumitsira mphepo yotentha chotchinga chimasunga tiyi kutali ndi utsi wobwera chifukwa cha kuyaka kwa malasha[26]. Pofuna kudziwa komwe kuli kodetsa, milingo ya AQ mumlengalenga idawunikidwa, zomwe zidapangitsa kuti pakhale kusiyana kwakukulu pakati pamisonkhano iwiriyi. Chifukwa chachikulu cha izi ndikuti malasha omwe amagwiritsidwa ntchito pokonza, kuyanika koyamba ndi kuyanikanso magawo angapangitse AQ pa kuyaka kosakwanira. Ma AQ awa adatulutsidwa mu tinthu tating'ono ta zolimba pambuyo pa kuyaka kwa malasha ndikumwazika mumlengalenga, kukweza kuchuluka kwa kuipitsidwa kwa AQ m'malo ochitira misonkhano[15]. M'kupita kwa nthawi, chifukwa cha malo akuluakulu komanso kuchuluka kwa tiyi, tiyi tiyi timakhala pamwamba pa masamba a tiyi, zomwe zimapangitsa kuti AQ achuluke. Choncho, kuyaka kwa malasha kunkaganiziridwa kuti ndiyo njira yaikulu yobweretsera kuipitsidwa kwa AQ pakupanga tiyi, ndipo utsi ndi umene umayambitsa kuipitsa.

Ponena za kukonza tiyi wa oolong, AQ idawonjezedwa pakukonzedwa ndi magwero onse otentha, koma kusiyana pakati pa magwero awiri otenthawa kunali kwakukulu. Zotsatira zake zidawonetsanso kuti malasha ngati gwero la kutentha adathandizira kwambiri kukulitsa mulingo wa AQ, ndipo kukonzako kudawonedwa ngati gawo lalikulu pakuwonjezera kuipitsidwa kwa AQ pakukonza tiyi wa oolong kutengera ma PF. Panthawi ya tiyi ya oolong yokhala ndi gasi-electric hybrid ngati gwero la kutentha, machitidwe a AQ level anali pansi pa 0.005 mg / kg, zomwe zinali zofanana ndi tiyi wobiriwira ndi magetsi, kutanthauza kuti mphamvu zoyera, monga magetsi ndi zachilengedwe. gasi, imatha kuchepetsa chiwopsezo chopanga zoyipitsa za AQ kuchokera pakukonzedwa.

Ponena za mayeso a zitsanzo, zotsatira zake zidawonetsa kuti kuipitsidwa kwa AQ kunali koyipa kwambiri mukamagwiritsa ntchito malasha ngati gwero la kutentha m'malo mwa magetsi, zomwe zitha kukhala chifukwa cha utsi woyaka malasha omwe amakumana ndi masamba a tiyi ndikuzungulira malo antchito. Komabe, ngakhale zinali zodziwikiratu kuti magetsi ndiye gwero la kutentha kwambiri panthawi yopangira tiyi, panalibe zonyansa za AQ muzinthu za tiyi zogwiritsa ntchito magetsi ngati gwero la kutentha. Mkhalidwewu ukuwoneka wofanana pang'ono ndi ntchito yomwe idasindikizidwa kale momwe machitidwe a 2- alkenals okhala ndi hydroquinones ndi benzoquinones adanenedwa ngati njira yamankhwala yomwe ingatheke [23], zifukwa za izi zidzafufuzidwa mu kafukufuku wamtsogolo.

MAPETO

Mu ntchitoyi, magwero omwe angayambitse kuwonongeka kwa AQ mu tiyi wobiriwira ndi oolong adatsimikiziridwa ndi kuyesa koyerekeza kutengera njira zowunikira za GC-MS/MS. Zomwe tapeza zimathandizira mwachindunji kuti gwero lalikulu loyipitsitsa la AQ lalitali linali utsi woyaka chifukwa cha kuyaka, komwe sikunangokhudza magawo okonzekera komanso kukhudza malo ochitira msonkhano. Mosiyana ndi magawo ogubuduza ndi ofota, pomwe kusintha kwa AQ kunali kosawoneka bwino, magawo omwe amakhudzidwa mwachindunji ndi malasha ndi nkhuni, monga kukonza, ndiye njira yayikulu yomwe kuipitsidwa kwa AQ kudakwera chifukwa cha kuchuluka kwa kulumikizana pakati pa tiyi. ndi utsi pa magawo amenewa. Chifukwa chake, mafuta oyera monga gasi ndi magetsi adalimbikitsidwa ngati gwero la kutentha pakukonza tiyi. Kuphatikiza apo, zotsatira zoyeserera zidawonetsanso kuti pakalibe utsi wopangidwa ndi kuyaka, palinso zinthu zina zomwe zimathandizira kutsata AQ panthawi yokonza tiyi, pomwe ma AQ ochepa adawonedwanso pamsonkhanowu ndi mafuta oyera, omwe ayenera kufufuzidwanso. mu kafukufuku wamtsogolo.

ZIDA NDI NJIRA

Reagents, mankhwala ndi zipangizo

Muyezo wa Anthraquinone (99.0%) unagulidwa kuchokera kwa Dr. Ehrenstorfer GmbH Company (Augsburg, Germany). D8-Anthraquinone yamkati (98.6%) idagulidwa ku C/D/N Isotopes (Quebec, Canada). Anhydrous sodium sulfate (Na2SO4) ndi magnesium sulfate (MgSO4) (Shanghai, China). Florisil idaperekedwa ndi Wenzhou Organic Chemical Company (Wenzhou, China). Pepala la mircro-glass fiber (90 mm) linagulidwa ku kampani ya Ahlstrom-munksjö (Helsinki, Finland).

Kukonzekera kwachitsanzo

Zitsanzo za tiyi wobiriwira zidakonzedwa ndi kukonza, kugudubuza, kuyanika koyamba ndi kuyanikanso (pogwiritsa ntchito zida zotsekeredwa), pomwe zitsanzo za tiyi za oolong zidakonzedwa ndikufota, kupanga zobiriwira (kugwedeza ndi kuyimirira masamba atsopano mosinthana), kukonza, kugudubuza, ndi kuyanika. Zitsanzo kuchokera pa sitepe iliyonse zinasonkhanitsidwa katatu pa 100g mutatha kusakaniza bwino. Zitsanzo zonse zinasungidwa pa -20 °C kuti zifufuzidwenso.

Zitsanzo za mpweya zinasonkhanitsidwa ndi pepala la fiber fiber (90 mm) pogwiritsa ntchito zitsanzo zapakati (PTS-100, Qingdao Laoshan Electronic Instrument Company, Qingdao, China) [27], ikuyenda pa 100 L / min kwa 4 h.

Zitsanzo zolimbitsidwa zidapangidwa ndi AQ pa 0.005 mg/kg, 0.010 mg/kg, 0.020 mg/kg kwa tiyi watsopano, pa 0.005 mg/kg, 0.020 mg/kg, 0.050 mg/kg pa tiyi wouma ndi 0.012 mg/kg (0.5 µg/m3 ya chitsanzo cha mpweya), 0.036 mg/kg (1.5 µg/m3 ya mpweya wocheperako), 0.072 mg/kg (3.0 µg/m3 ya chitsanzo cha mpweya) pa pepala losefera magalasi, motsatana. Pambuyo pogwedeza bwino, zitsanzo zonse zinasiyidwa kwa maola 12, ndikutsatiridwa ndi masitepe ochotsa ndi kuyeretsa.

Chinyezicho chinapezedwa potenga 20 g ya chitsanzo mutatha kusakaniza sitepe iliyonse, kutentha pa 105 ° C kwa 1 h, kenako kulemera ndi kubwereza katatu ndi kutenga mtengo wapakati ndikugawaniza ndi kulemera kusanayambe kutentha.

Kuchotsa zitsanzo ndi kuyeretsa

Chitsanzo cha tiyi: Kuchotsa ndi kuyeretsedwa kwa AQ kuchokera ku zitsanzo za tiyi kunachitika kutengera njira yofalitsidwa ndi Wang et al. ndi zosintha zingapo [21]. Mwachidule, 1.5 g ya zitsanzo za tiyi idasakanizidwa koyamba ndi 30 μL D8-AQ (2 mg / kg) ndikusiyidwa kuti iyime kwa mphindi 30, kenako imasakanizidwa bwino ndi 1.5 mL yamadzi oyeretsedwa ndikusiya kuyimirira kwa mphindi 30. 15 mL 20% acetone mu n-hexane anawonjezera kuti tiyi zitsanzo ndi sonicated 15 min. Ndiye zitsanzo zinali vortexed ndi 1.0 g MgSO4 kwa 30 s, ndi centrifuged kwa 5 min, pa 11,000 rpm. Pambuyo posamutsidwa ku 100 mL zoboola zooneka ngati peyala, 10 mL ya gawo lapamwamba la organic idasinthidwa kukhala nthunzi pafupifupi kuuma pansi pa vacuum pa 37 °C. 5 mL 2.5% acetone mu n-hexane adasungunulanso chotsitsacho mu fulasiki yooneka ngati peyala kuti ayeretsedwe. Mzati wagalasi (10 cm × 0,8 cm) unali kuchokera pansi mpaka pamwamba pa galasi ubweya ndi 2g florisil, amene anali pakati pa zigawo ziwiri za 2 cm Na2SO4. Kenako 5 ml ya 2.5% acetone mu n-hexane adatsuka ndime. Pambuyo pokweza yankho losungunukanso, AQ idasinthidwa katatu ndi 5 mL, 10 mL, 10 mL ya 2.5% acetone mu n-hexane. Zosakaniza zophatikizidwazo zinasamutsidwa ku ma flasks ooneka ngati mapeyala ndipo amasanduka nthunzi pafupifupi kuuma pansi pa vacuum pa 37 ° C. Zotsalira zoumazo zidakonzedwanso ndi 1 mL ya 2.5% acetone mu hexane ndikutsatiridwa ndi kusefera kudzera pa fyuluta ya 0.22 µm pore size. Kenako yankho lokonzedwanso linasakanizidwa ndi acetonitrile pamlingo wa 1: 1. Kutsatira sitepe yogwedezeka, subnatant idagwiritsidwa ntchito posanthula GC-MS/MS.

Zitsanzo za mpweya: Theka la pepala la fiber, lodontha ndi 18 μL d8-AQ (2 mg/kg), linamizidwa mu 15 mL ya 20% acetone mu n-hexane, kenako sonicated kwa 15 min. Gawo lachilengedwe linalekanitsidwa ndi centrifugation pa 11,000 rpm kwa 5 min ndipo gawo lonse lapamwamba linachotsedwa mu botolo lopangidwa ndi peyala. Magawo onse achilengedwe adasinthidwa kukhala nthunzi pafupifupi kuuma pansi pa vacuum pa 37 ° C. 5 ml ya 2.5% ya acetone mu hexane idasungunulanso zowonjezera kuti ziyeretsedwe mofanana ndi zitsanzo za tiyi.

Kusanthula kwa GC-MS/MS

Varian 450 gas chromatograph yokhala ndi Varian 300 tandem mass detector (Varian, Walnut Creek, CA, USA) idagwiritsidwa ntchito kusanthula AQ ndi pulogalamu ya MS WorkStation version 6.9.3. Varian Factor Four capillary column VF-5ms (30 m × 0.25 mm × 0.25 μm) idagwiritsidwa ntchito pakupatukana kwa chromatographic. Mpweya wonyamulira, helium (> 99.999%), unayikidwa pa mlingo wokhazikika wa 1.0 mL / min ndi kugunda kwa mpweya wa Argon (> 99.999%). Kutentha kwa uvuni kunayamba kuchokera ku 80 ° C ndikusungidwa kwa mphindi imodzi; chinawonjezeka pa 15 ° C / min mpaka 240 ° C, kenako chinafika 260 ° C pa 20 ° C / min ndikugwira kwa 5min. Kutentha kwa gwero la ion kunali 210 ° C, komanso kutentha kwa mzere wotumizira wa 280 ° C. Kuchuluka kwa jakisoni kunali 1.0 μL. Mikhalidwe ya MRM ikuwonetsedwa mu Table 3.

Agilent 8890 gas chromatograph yokhala ndi Agilent 7000D triple quadrupole mass spectrometer (Agilent, Stevens Creek, CA, USA) idagwiritsidwa ntchito kusanthula kuyeretsedwa ndi pulogalamu ya MassHunter version 10.1. Agilent J&W HP-5ms GC Column (30 m × 0.25 mm × 0.25 μm) idagwiritsidwa ntchito pakulekanitsa chromatographic. Mpweya wonyamulira, Helium (> 99.999%), adayikidwa pamlingo wokhazikika wa 2.25 mL / min ndi kugunda kwa mpweya wa Nitrogen (> 99.999%). Kutentha kwa gwero la EI ion kunasinthidwa pa 280 ° C, mofanana ndi kutentha kwa mzere wotumizira. Kutentha kwa uvuni kunayamba kuchokera ku 80 ° C ndipo kunachitika kwa mphindi 5; kukwezedwa ndi 15 ° C / min mpaka 240 ° C, kenako kufika 280 ° C pa 25 ° C / min ndikusungidwa kwa 5 min. Mikhalidwe ya MRM ikuwonetsedwa mu Table 3.

Kusanthula kwachiwerengero
Zomwe zili mu AQ m'masamba atsopano zidakonzedwa kuti ziume zowuma pozigawa ndi chinyezi kuti zifananize ndi kusanthula milingo ya AQ pakukonza.

Zosintha za AQ mu zitsanzo za tiyi zidawunikidwa ndi Microsoft Excel software ndi IBM SPSS Statistics 20.

Processing factor idagwiritsidwa ntchito kufotokoza kusintha kwa AQ panthawi yokonza tiyi. PF = Rl/Rf , kumene Rf ndi mlingo wa AQ musanayambe sitepe yokonza ndipo Rl ndi mlingo wa AQ pambuyo pa sitepe yokonza. PF ikuwonetsa kuchepa (PF <1) kapena kuwonjezeka (PF> 1) muzotsalira za AQ panthawi yokonzekera.

ME imasonyeza kuchepa (ME <1) kapena kuwonjezeka (ME> 1) poyankha zida zowunikira, zomwe zimachokera ku chiŵerengero cha otsetsereka a calibration mu matrix ndi zosungunulira motere:

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

Kumene slopematrix ndi malo otsetsereka okhotakhota mu zosungunulira zofananira ndi matrix, slopesolvent ndi malo otsetsereka a calibration curve mu zosungunulira.

KUYAMIKIRA
Ntchitoyi idathandizidwa ndi Science and Technology Major Project ku Zhejiang Province (2015C12001) ndi National Science Foundation of China (42007354).
Kusemphana kwa chidwi
Olembawo akulengeza kuti alibe mkangano wa chidwi.
Ufulu ndi zilolezo
Copyright: © 2022 wolemba(a). Exclusive Licensee Maximum Academic Press, Fayetteville, GA. Nkhaniyi ndi nkhani yotseguka yoperekedwa pansi pa Creative Commons Attribution License (CC BY 4.0), pitani ku https://creativecommons.org/licenses/by/4.0/.
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Za nkhaniyi
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