-Catshangwa
I-9,10-Anthraquinone (AQ) iyona engcolisa ngengozi enokwenzeka ye-carcinogenic futhi yenzeka etiyeni emhlabeni wonke. Umkhawulo we-regimue we-AQ (MRL) we-AQ etiye e-European Union (EU) ngu-0.02 mg / kg. Imithombo engenzeka ye-AQ ekucutshungweni kwetiye kanye nezigaba eziphambili zokuvela kwayo kuphenywe ngokususelwa endleleni yokuhlaziya ye-AQ eguquliwe kanye negesi i-chromatography (i-GC-MS / MS Spectrometry (GC-MS / MS Spectrometry (GC-MS / MS) Ukuhlaziywa. Uma kuqhathaniswa nogesi njengomthombo wokushisa ekucutshungulweni kwetiye eliluhlaza, i-AQ ikhuphuke ngamahlandla angama-4,3 kuye kwayi-23.9 ekusebenzeni kwetiye kanye nomthombo wokushisa, ngenkathi izinga le-0.02 mg liphindeke kathathu. Umkhuba ofanayo waqashelwa ku-Ooong Tea Ukucubungula ngaphansi kokushisa kwamalahle. Izinyathelo ezinokuxhumana ngqo phakathi kwamaqabunga etiye kanye nentukuthelo, njengokulungiswa nokomisa, kubhekwa njengezinyathelo eziphambili zokukhiqizwa kwe-AQ ekukhiqizeni itiye. Amazinga we-AQ akhuphuke ngesikhashana sokuxhumana, ephakamisa ukuthi amazinga aphezulu we-AQ Pollotant eTea angasuselwa kumathumbu adalwa amalahle nokuhlangana. Amasampula angamashumi amane avela kuma-workshop ahlukene anogesi noma amalahle njengoba imithombo yokushisa yahlaziywa, isukela ku-50.0% -85.0% no-5.0% -35.0% ukuthola amanani e-AQ. Ngaphezu kwalokho, okuqukethwe okuphezulu kwe-AQ kwe-0.064 mg / kg kwaqashelwa kumkhiqizo wetiye ngamalahle njengoba umthombo wokushisa, okukhombisa ukuthi amazinga aphezulu okungcoliswa kwe-AQ emikhiqizweni yetiye kungenzeka afake isandla ngamalahle.
Amagama agqamile: 9,10-Anthraquinone, ukucubungula itiye, amalahle, umthombo wokungcola
Ukuqalisa
Kwenziwe itiye emacembe eShren shrub Camellia Sounsis (L.) O. Kuntze, kungenye yeziphuzo ezithandwa kakhulu emhlabeni wonke ngenxa yokunambitheka kwayo okuqabulayo kanye nezinzuzo zezempilo. Ngo-2020 emhlabeni jikelele, ukukhiqizwa kwetiye kwanda kufinyelela kumathani ama-metric ayizigidi ezingama-5,972, okwakuyinto ephindwe kabili eminyakeni engama-20 edlule [1]. Kususelwa ezindleleni ezahlukahlukene zokucubungula, kunezinhlobo eziyisithupha eziphambili zetiye, kufaka phakathi itiye eliluhlaza, itiye elimnyama, itiye elimnyama, itiye elimnyama, itiye elimhlophe, itiye elimhlophe netiye elimhlophe netiye elimhlophe netiye elimhlophe netiye elimhlophe netiye [itiye elimhlophe. Ukuqinisekisa ikhwalithi nokuphepha kwemikhiqizo, kubaluleke kakhulu ukuqapha amazinga okungcola futhi uchaze umsuka.

Ukuhlonza imithombo yezinto ezingcolisayo, njengezinsalela zokubulala izinambuzane, izinsimbi ezisindayo nokunye ukungcola okufana ne-polycyclic aromatic hydrocarbons (PAHS), yisinyathelo sokuqala sokulawula ukungcoliswa. Ukufafaza okuqondile kwamakhemikhali okwenziwa emasimini itiye, kanye nomoya odonsa umoya okubangelwa ukusebenza eduze kwezingadi zetiye, kungumthombo oyinhloko wezinsalela zokubulala izinambuzane etiye [4]. Izinsimbi ezisindayo zinganqwabelana itiye futhi ziholele ubuthi, ezithathwe ikakhulu emhlabathini, umanyolo kanye nomoya ongu-5-7]. Ngokuqondene nokunye ukungcoliswa okuvela kungazelelwe etiyeni, bekunzima impela ukukhomba ngenxa yezinqubo eziyinkimbinkimbi zokwenziwa kwetiye tea kufaka phakathi ukutshala, ukucubungula, iphakheji, ukugcinwa nokuhamba. Ama-pahs etiyeni aqhamuka ekugcinweni kwamandla okuphela kwemoto kanye nokuhlanganiswa kwamafutha asetshenziswa ngesikhathi sokucutshungulwa kwamaqabunga etiye, njengowokufa amalahle namalahle [8-10].

Ngesikhathi sokuhlanganiswa kwamalahle kanye nokuvuselelwa kwezinkuni, ukungcola okunjenge-carbon oxides kwakhiwa [11]. Ngenxa yalokhu, kutholakala ukuthi izinsalela zalezi zingcoliswa ezingenhla zivele emikhiqizweni esetshenzisiwe, njengokusanhlamvu, isitoko esibhemayo kanye nezinhlanzi zekati, lapho kusongela impilo yabantu [12,13]. Ama-pahs abangelwa ukuvutha asuselwa ekuthambekeni kwama-pahs aqukethe ama-fuels uqobo, ukubola okushisa okuphezulu kwamakhompiyutha amnandi kanye nokusabela okuhlanganisiwe phakathi kwama-radicals wamahhala [14]. Ukushisa kokuhlanganisa, isikhathi, kanye nokuqukethwe kwe-oxygen kuyizinto ezibalulekile ezithinta ukuguqulwa kwe-PAHs. Ngokunyuka kwamazinga okushisa, okuqukethwe kwe-pahs kukhuphuke okokuqala kwabe sekuncipha, futhi inani eliphakeme lenzeke ngo-800 ° C; Okuqukethwe kwe-PAHS kwehle kakhulu ukulandelela isikhathi sokuhlangana esandayo lapho kungaphansi komkhawulo obizwa nge-'Ving Time ', kepha ukuphuma kwe-oxygen' kuncishiswe kakhulu, kepha i-oxivation engaphelele ibizokhiqiza i-opah nezinye izithonjana [15-17].

I-9,10-Anthraquinone (AQ, CAS: 84-65-1, Fig. 1), i-oksijini equkethe okususelwa kuma-pahs [18], iqukethe imijikelezo emithathu evunyelwe. Yafakwa kuhlu njenge-carcinogen engenzeka (iqembu 2b) yi-International Agency ukuze ucwaninge ngomdlavuza ngo-2014 [19]. I-AQ ingavuselela eTopoisomerase II Cleavage Complex futhi ivimbela i-hydrolysis ye-adenosine trisosphate II, okubangela ukuvezwa okuphezulu kwe-AQ, okusho ukuthi ukuvezwa okuphezulu kwe-AQ kuholela ekulimaleni kwe-AQ, okungu-20]. Njengemiphumela emibi empilweni yabantu, umkhawulo we-AQ omkhulu we-Recidence umkhawulo (MRL) we-0.02 mg / kg wahlelwa etiyeni yi-European Union. Ngokwezifundo zethu zangaphambili, kwaphakanyiswa imali efakiwe njengomthombo oyinhloko ngesikhathi sokutshala kwetiye [21]. Futhi, ngokuya ngemiphumela yokuhlola ekucutshungweni kwetiye okuluhlaza okotshani kwe-Indonesia, kusobala, kusobala ukuthi izinga le-AQ lishintshe kakhulu futhi intuthu emishini ecubungula yaphakanyiswa njengenye yezizathu eziphambili [22]. Kodwa-ke, umsuka onembile we-AQ ekucutshungweni kwetiye wasaqhubeka engenakuqhathaniswa, yize amanye ama-hypotheses e-AQ Chemical Payaway aphakanyiswa [okubonisa ukuthi kubaluleke kakhulu ukuthola izici ezibalulekile ezithinta izinga le-AQ.

Umdwebo 1. Ifomula yamakhemikhali ye-AQ.

Njengoba kunikezwe ucwaningo ngokwakhiwa kwe-AQ ngesikhathi sokuhlanganiswa kwamalahle kanye nengozi engaba khona yamafutha ekusebenzeni kwetiye, kuwusizo ukucubungula umsuka oqondile, okuwusizo iphethini ye-AQ kanye ne-degree yokungcoliswa kwe-AQ ekuguqukeni kweTEA.

Umphumela
Ukuqinisekiswa kwendlela
Uma kuqhathaniswa nesifundo sethu sangaphambilini [21], inqubo yokukhiya uketshezi yayihlanganiswa ngaphambi kokujova ku-GC-MS / MS ukuze ithuthukise ukuzwela nokugcina izitatimende zensimbi. Ku-Fig 2b, indlela ethuthukisiwe ikhombisa ukuthuthuka okukhulu ekuhlanzweni kwesampula, i-solvent yaba lula ngombala. Ku-Fig 2a, i-scan ephelele (50-350 m / z) eboniswe ngemuva kokuhlanzwa, umugqa wesisekelo we-MS Spectrum uncishisiwe kusobala ukuthi ama-chromatographic aphezulu atholakala, okukhombisa ukuthi inani elikhulu lezinhlanganisela zokuphazamiseka zisuswe ngemuva kokukhishwa okuwuketshezi.

Umdwebo 2. (A) Ukuhlola okugcwele kwesampula ngaphambi nangemva kokuhlanzwa. (b) Umphumela wokuhlanza wendlela ethuthukisiwe.
Ukuqinisekiswa kwendlela, kufaka phakathi ukufutheka, ukululama, umkhawulo we-quach (loq) kanye ne-matrix umphumela (me), kukhonjiswe kusuka ku-0.998, ku-solvent yetiye kanye no-ailet ekhasini elingu-0.5 kuya ku-8 μg / m3.

Ukubuyiselwa kwe-AQ kuhlolwe ekugxiliseni okuthathu okwenziwe spiked phakathi kwetiye elomile neli-0.005, 0.05 mg / 0.55 mg / 0.5, 0.01, 0.5, 1.5, 1,5, 3 μg / m3). Ukubuyiselwa kwe-AQ etiyeni kusuka ku-77.78% kuya ku-113.02% etiyeni elomile futhi kusuka ku-96.52% kuya ku-125.69% kumahlumela wetiye, nge-RSD% ephansi kune-15%. Ukubuyiselwa kwe-AQ kumasampula e-AIR aqhamuke ku-78.47% kuya ku-117.06% nge-RSD% ngaphansi kwama-20% ngaphansi kwama-20%. Ukuhlushwa okuphansi okuphansi kukhonjwe njenge-loq, okwakungu-0.005 mg / kg, 0.005 mg / kg kanye 0.5 μg / amasampula etiye kanye nomoya, ngokulandelana. Njengoba kubhalwe kuThebula 1, i-matrix yetiye elomile kanye namahlumela amahlumela kancane akhulisa impendulo ye-AQ, okuholela kimi engu-109.0% no-110.9%. Ngokuqondene ne-matrix yamasampula endiza, kimi kwakungu-196.1%.

Amazinga we-AQ ngesikhathi sokucubungula i-Green Tea
Ngenhloso yokuthola imiphumela yemithombo eshibhile ehlukene ethangeni nasekusetshenzisweni kwamaqabunga amasha ahlukaniswe ngamaqembu amabili athile futhi acutshungulwa ngokwahlukana ezindaweni ezimbili zokucubungula ebhizinisini elifanayo. Elinye iqembu lanikezwa ugesi, kanti elinye ngamalahle.

Njengoba kukhonjisiwe ku-Fig. 3, izinga le-AQ elinogesi njengoba umthombo wokushisa wasuka ku-0,008 kuye ku-0.013 mg / kg. Ngesikhathi sokulungiswa kwenqubo, isigaxa samaqabunga etiye esibangelwa ukucubungula ebhodweni ngokushisa okuphezulu okuholele ekunyuseni okuphezulu kwe-9.5% e-AQ. Ngemuva kwalokho, izinga le-AQ lasala ngesikhathi senqubo yokugoqa naphezu kokulahleka kwejusi, liphakamisa ukuthi izinqubo zomzimba zingaphazamisi izinga le-AQ ekucutshungweni kwetiye. Ngemuva kwezinyathelo zokuqala zokomisa, izinga le-AQ lenyuke kancane kusuka ku-0.010 kuya ku-0.012 mg / kg, laqhubeka nokukhuphuka ku-0.013 mg / kg kuze kube sekupheleni kokumiswa kabusha. I-PFS, ekhombisa kakhulu ukuhlukahluka esigabeni ngasinye, kwakungu-1.10, 1.03, 1.24, 1.08 ekuhlelweni, ukugingqa, ukuyomisa okokuqala kanye nokomisa kabusha, ngokulandelana. Imiphumela yama-PFS iphakamise ukuthi ukucubungula ngaphansi kwamandla kagesi kwaba nomphumela omncane emazingeni e-AQ etiye.

Umdwebo 3. Izinga le-AQ ngesikhathi sokusebenza kwetiye eliluhlaza osebenza ngogesi namalahle njengemithombo yokushisa.
Endabeni yamalahle njengomthombo wokushisa, okuqukethwe kwe-AQ kwanda kakhulu ngesikhathi sokucutshungulwa kwetiye, ukudonsa kusuka ku-0.008 kuya ku-0.038 mg / kg. I-338.9% I-AQ yandiswa kwinqubo yokulungiswa, ifinyelela ku-0.037 mg / kg, okudlula kude i-MRL ye-0.02 mg / kg isethwe yi-European Union. Ngesikhathi sokugoqa, izinga le-AQ lisenyuswe ngo-5.8% yize likude nomshini wokuhlelwa. Ekuqaleni kokomiswa nokuhlelwa kabusha, okuqukethwe kwe-AQ kwakhuphuka kancane noma kwehle kancane. Ama-PFs asebenzisa amalahle njengoba umthombo wokushisa ocingeni, ukugingqa ukomisa kokuqala nokumisa kabusha kwakungu-4.39, 1.05, 0.93, kanye ne-1.05, ngokulandelana.

Ukuqhubeka nokunquma ubudlelwano phakathi kokuhlanganiswa kwamalahle kanye nokungcoliswa kwe-AQ, izindaba ezimisiwe (i-PMS) emoyeni ocwaningweni lokuwohloka ngaphansi kwemithombo yokushisa yaqoqwa ngo-2.98 μg / M3, obekungaphezulu kathathu.

Umdwebo 4. Amazinga we-AQ emvelweni enogesi namalahle njengomthombo wokushisa. * Ibonisa umehluko obalulekile kumazinga we-AQ kumasampula (P <0.05).

Amazinga we-AQ ngesikhathi se-Oolong Tea ecubungula itiye le-Oolong Tea, elikhiqizwa ikakhulu eFujian naseTaiwan, uhlobo lwetiye elivutha ngokwengxenye. Ukuqhubeka nokunquma izinyathelo eziphambili zokwanda kweleveli ye-AQ kanye nemiphumela yamafutha ahlukene, i-batch efanayo yamaqabunga amasha yenziwa ngetiye le-ooong ne-hybrid yemvelo yemvelo njengemithombo yokushisa, ngasikhathi sinye. Amazinga we-AQ ecubungula le-Oolong Tea esebenzisa imithombo eshibhile ehlukene akhonjiswe ku-Fig. 5. Ukucutshungulwa kwetiye kwe-Oool

Umdwebo 5. Ileveli ye-AQ ngesikhathi sokulungiswa kwetiye kwe-Oool

Ngamalahle njengomthombo wokushisa, amazinga we-AQ ezitebhisini ezimbili zokuqala, abune futhi enza okuluhlaza, empeleni kwakufana nokuhlanganiswa kwegesi yemvelo kagesi. Kodwa-ke, izinqubo ezalandela kuze kube yilapho ukulungiswa kukhombisa igebe elikhulisa kancane kancane, lapho izinga le-AQ liqhamuka ku-0,004 kuye ku-0.023 MG / KG. Izinga esiteji sokugibela esigcwele sehle saya ku-0.018 mg / kg, okungenzeka ngenxa yokulahleka kwejusi le-TEA elisebenzisa ezinye zezinto ezingcolisayo ze-AQ. Ngemuva kwesiteji sokugoqa, izinga esigabeni sokomisa lenyuka liye ku-0.027 mg / kg. Ngokubuna, ukwenza okuluhlaza okotshani, ukulungisa, ukugoqa okugcwele nokomiswa, ama-PFs ayengu-2.81, 1.32, 5.66, 0.78, no-1.50, ngokulandelana.

Ukuvela kwe-AQ emikhiqizweni yetiye ngemithombo ehlukene yokushisa

Ukunquma imiphumela ekuqukethwe kwe-AQ yetiye enemithombo ehlukene yokushisa, amasampula etiye ama-40 avela kuma-Workshops noma amalahle atholakale esebenzisa amanani aphezulu we-AQ. Ukuhlanganiswa, kanye nesilinganiso sama-35.0% abonwa kumasampula amalahle. Ngokubona kakhulu, ugesi wayenomenyezeli ophansi kakhulu kanye namanani aphansi angu-56.4% no-7.7% ngokulandelana, ngokuqukethwe okuphezulu kwe-0.020 mg / kg.

Ukukhuluma

Kususelwa kuma-PF ngesikhathi sokulungiswa nezinhlobo ezimbili zemithombo yokushisa, bekucacile ukuthi ukulungiswa kwawo kwakuyisinyathelo esiyinhloko sokuba sekwanda kwamazinga e-AQ nokusebenza ngaphansi kwamandla kagesi kwaba nomphumela omncane kokuqukethwe kwe-AQ. Ngesikhathi sokucutshungulwa kwetiye eluhlaza, ukuhlanganiswa kwamalahle kukhiqize intuthu eminingi enqubweni yokulungiswa kuqhathaniswa nenqubo yokufudumala kagesi, okukhombisa ukuthi mhlawumbe ama-fumes ayengumthombo wokungcoliswa kwetiye kusuka ekuxhumaneni kwamasampula wetiye [25]. Ukwanda okuncane kokuqukethwe kwe-AQ ngesikhathi sokugoqa kuphakamise ukuthi ama-fumes angenzeka ukuthi ukuhlanganiswa kwamalahle akuzange kuthinte kuphela izinga le-AQ kuphela ngesikhathi sesinyathelo sokulungiswa, kepha nasendaweni ecubungula ngenxa yokufakwa komkhathi. Amalahle abuye asetshenziswe njengomthombo wokushisa okomeni kokuqala nokomisa kabusha, kepha kulezi zinyathelo ezimbili okuqukethwe kwe-AQ kukhuphuke kancane noma kwehle kancane. Lokhu kungahle kuchazwe ngeqiniso lokuthi owomile oshisayo oshisayo wagcina itiye kude ne-fumes ebangelwa ukuhlanganiswa kwamalahle [26]. Ukuze unqume umthombo ongcolile, amazinga we-AQ emkhathini ahlaziywa, ahole kwigebe elibalulekile phakathi kwalezi zindawo zokusebenzela zomishozo ezimbili. Isizathu esiyinhloko salokhu ukuthi amalahle asetshenziswe ocingweni, ukumiswa kokuqala kokumiswa nokuphinda akhiqize i-AQ ngesikhathi sokuhlangana okungaphelele. Lezi zi-AQ zibe seziduduzwa ngezinhlayiya ezincane zama-solids ngemuva kokuhlanganiswa kwamalahle futhi zihlakazeke emoyeni, ziphakamise amazinga okungcoliswa kwe-AQ endaweni yokusebenzela indawo yokusebenzela [15]. Ngokuhamba kwesikhathi, ngenxa yendawo enkulu engaphezulu komhlaba kanye namandla e-adcorption wetiye, lezi zinhlaka zale zixazululwa ebusweni bamaqabunga etiye, okuholela ekwandeni kwe-AQ ekukhiqizeni. Ngakho-ke, ukuhlanganiswa kwamalahle kwakucatshangwa ukuthi kuyindlela eyinhloko eholela ekungcoleni ngokweqile kwe-AQ ekucutshungweni kwetiye, ngentukuthelo engumthombo wokungcola.

Ngokuqondene nokucutshungulwa kwetiye ye-Oolong, i-AQ yandiswa ngaphansi kokucubungula ngemithombo yokushisa, kepha umehluko phakathi kwemithombo emibili yokushisa wawubalulekile. Imiphumela ibuye yaphakamisa ukuthi amalahle njengoba umthombo wokushisa wadlala indima enkulu ekwandiseni izinga le-AQ ekhuphukayo, futhi ukulungiswa kwathathwa njengesinyathelo esikhulu sokwandisa ukungcoliswa kwe-AQ kwe-AQ okusekelwe kuma-PF. Ngesikhathi sokucutshungulwa kwetiye kwe-oolong nge-hybrid yemvelo yomthombo kagesi njengomthombo wokushisa, umkhuba we-AQ level wawumisa ngaphansi kwetiye eliluhlaza ogesi, ophakamisa ukuthi ugesi kanye negesi yemvelo, anganciphisa ubungozi bokukhiqiza ukungcoliswa kwe-AQ.

Ngokuqondene nokuhlolwa kwesampula, imiphumela yabonisa ukuthi isimo se-contaminannion ye-AQ sasisibi kakhulu lapho sisebenzisa amalahle njengomthombo wokushisa kunogesi, okungenzeka ngenxa yemifudlana kusuka kugesi kuhlangana namaqabunga etiye kanye nokuhamba ngezinyawo endaweni yokusebenza. Kodwa-ke, yize bekusobala ukuthi ugesi kwakuwumthombo wokushisa ohlanzekile kakhulu ngesikhathi sokulungiswa kwetiye, bekusekhona ukungcola kwe-AQ emikhiqizweni yetiye kusetshenziswa ugesi njengomthombo wokushisa. Lesi simo sibonakala sifana kancane nomsebenzi owawushicilelwe ngaphambili lapho ukusabela kwama-alkrkwane nama-hydroquones kanye ne-benzoququones kuphakanyiswe njengendlela engaba khona yamakhemikhali [23], izizathu zalokhu zizophenywa ngocwaningo oluzayo.

Iziphetho

Kulomsebenzi, imithombo esenzeka ekungcoleni i-AQ eTreen and Oolong Tea yaqinisekiswa ngokuhlolwa kokuqhathanisa ngokusekelwe izindlela ezithuthukisiwe ze-GC-MS / MS. Ukutholwa kwethu kuxhase ngqo ukuthi umthombo ongokomhloli ophakeme wamazinga aphezulu we-AQ wayebangelwa yi-combustion, ngaphandle kokuthi athinte kuphela izigaba zokucubungula kodwa futhi athinte izindawo zokusebenzela zokusebenzela. Ngokungafani nezigaba zokugoqa nezibusayo, lapho izinguquko ezikuleveli ze-AQ zazingenangqondo, izigaba ezinokuzibandakanya okuqondile kwamalahle nezinkuni, ziyinqubo enkulu lapho i-AQ Comporation lapho kuvela khona inani lokuxhumana phakathi kwalezi zigaba. Ngakho-ke, amafutha ahlanzekile anjengegesi yemvelo anconywa njengomthombo wokushisa ekucutshungweni kwetiye. Ngokwengeziwe, imiphumela yokuhlola ibuye ikhombise ukuthi uma kungekho okubi okwenziwe yi-combustion, kunezinye izici ezibangela ukulandelela i-AQ ngesikhathi sokusebenza kwetiye, okufanele kubhekwe ngokuqhubekayo ocwaningweni oluhlanzekile.

IZIMPAHLA NEZINDLELA

Ama-reagents, amakhemikhali nezinto zokwakha

I-Anthraquicone ejwayelekile (99.0%) yathengwa kuDkt Ehrenstorfer GmbHH Inkampani (Augsburg, Germany). I-D8-anthraquequone ejwayelekile (98.6%) yathengwa kusuka ku-C / D / N ISTOTOPES (Quebec, eCanada). I-Anhydrous Sodium Sulfate (NA1SHO4) kanye ne-Magnesium Sulfate (MGSO4) (SHANGHA4, China). IFlorisil yanikezwa yiWenzhou Organic Chemical Company (Wenzhou, China). Iphepha le-Mircro-Glass Fiber (90 mm) lithengwe ku-Ahlstrom-Munksjö Company (Helsinki, Finland).

Ukulungiswa kwesampula

Amasampula etiye e-Green acutshungulwa ngokulungiswa, ukugoqa, ukomisa okokuqala nokumisa kabusha (kusetshenziswa amasampula afakiwe), ngenkathi amaqabunga e-oolong itiye), ngenkathi amaqabunga amasha afakiwe), enza amaqabunga amasha agcwele), ulungisake, ugobe, ukomisa. Amasampula esigabeni ngasinye aqoqwa kathathu ku-100g ngemuva kokuxubana okuphelele. Onke amasampula agcinwe ku-20 ° C ukuze ahlaziywe okunye.

Amasampula e-AIR aqoqwe ngephepha le-fiber ye-Glass (90 mm) esebenzisa ama-sampler aphakathi nendawo (ama-PTS-100, qingdao Laoshan Ithuluzi Wezinsimbi, qingdao, China) [27], egijima ku-4 h.

Amasampula aqinisiwe ahlelwe nge-AQ ku-0.005 MG / KG, 0.010 MG / KG, 0.020 MG / KG, 0.050 MG / KG, 0.050 MG / KG, 0.505 / M3 ngesampula yomoya), 0.036 I-MG / KG (1.5 μg / m3 ye-Air Smaple), 0.072 MG / KG (3.0 μg / m3 ngesampula yomoya) yephepha lokuhlunga lengilazi, ngokulandelana. Ngemuva kokuthuthumela kahle, wonke amasampula ashiywe ngo-12 h, alandelwa yizinyathelo zokuhlanza nezinyathelo zokuhlanza.

Ukuqukethwe komswakama kutholwe ngokuthatha amasampula angama-20 g wesampula ngemuva kokuxuba isinyathelo ngasinye, ukufudumeza ku-105 ° C nge-1 h, bese unesisindo futhi uphindaphindeke kathathu futhi uwuhlukanise ngesisindo ngaphambi kokushisa.

Ukukhishwa kwesampula kanye nokuhlanza

Isampula yetiye: Ukukhishwa kanye nokuhlanza kwe-AQ kusuka kumasampula etiye kwenziwa ngokususelwa kwindlela eshicilelwe kusuka ku-wang et al. ngokuvumelana okuningana [21]. Kafushane nje, 1.5 g amasampula etiye ahlanganiswe okokuqala ne-30 μl d8-aq (2 mg / kg) futhi kwesobunxele ukumela amanzi angama-30, bese exubene kahle namaminithi angu-1.5 ml. I-15 ml 20% acetone e-N-Hexane yengezwe kumasampula etiye futhi inenhlonipho imizuzu eyi-15. Lapho-ke amasampula afakwe nge-1.0 g mgso4 ngama-30 s, futhi centrifugud angu-5 imizuzu, ku-11,000 RPM. Ngemuva kokuthuthelwa kuma-flasks angu-100 ml abunjwe ngo-10, i-10 ml yesigaba esingenhla se-organic yavele yavele isono ngaphansi kwe-vacuum ngaphansi kwe-37 ° C. I-5 ml 2.5% Acetone e-N-Hexane iphinde yakhipha okukhishwe ngama-flasks abunjwe ngopele ukuze ahlanjululwe. Ikholomu yengilazi (10 cm × 0,8 cm) yayiqukethe kusuka phansi kuya phezulu kwenye yoboya bengilazi kanye ne-2g florisil, eyayiphakathi kwezendlalelo ezimbili ze-2 cm NA1SO4. Ngemuva kwalokho i-5 ml ka-2,5% acetone e-N-Hexane Preswashed the coloum. Ngemuva kokulayisha isixazululo esinqunyelwe kabusha, i-AQ yaqoshwa kathathu nge-5 ml, 10 ml, 10 ml ka-2,5% acetone e-N-Hechane. Abakwa-Hlate ahlanganisiwe badluliselwe emapholini abunjwe ngopele futhi bavele bacishe boma ngaphansi kwe-vacuum ku-37 ° C. Izinsalela ezomisiwe ziphinde zavulwa nge-1 ml ka-2,5% acetone eHexane elandelwa ukugcwala ngohlobo lwe-Filtration ngesihlungi se-0.22 μm pore usayizi. Ngemuva kwalokho isixazululo esivuthiwe sahlanganiswa ne-acetonitrile ngesilinganiso sevolumu ye-1: 1. Ngemuva kwesinyathelo esishukumisayo, isigatshana sasisetshenziselwa ukuhlaziya kwe-GC-MS / MS.

Isampula yomoya: Ingxenye yephepha le-fiber, edonswe nge-18 μl d8-aq (2 mg / kg), yacwiliswa ku-15 ml ka-20% acetone e-N-Heste. Isigaba se-organic sahlukaniswa nge-centrifugation ku-11,000 RPM ngamaminithi ayi-5 nalo lonke ungqimba olungenhla lwasuswa ku-flask enobumba. Zonke izigaba ze-organic zazihanjiswa cishe ukuze zome ngaphansi kwe-vacuum ku-37 ° C. I-5 ml ka-2,5% acetone eHexane iphinde yakhipha izifinyezo zokuhlanzwa ngendlela efanayo nakumasampula etiye.

Ukuhlaziywa kwe-GC-MS / MS

I-Varian 450 igesi i-Chromatographs ifakwe umtshina we-varian 300 Tandem Masstector (Varian, Walnut Creek, CA, USA) wasetshenziselwa ukucubungula i-AQ Workstation version 6.9.3 Software. I-Varian Factor ezine ikholamu yekholamu VF-5ms (30 m × 0,25 mm × 0.25 μm) isetshenziselwe ukwehlukaniswa kwe-chromatomatographic. I-Carrier Gream, Helium (> 99.999%), yahlelwa ngesilinganiso sokugeleza esingaguquki se-1.0 ml / min nge-collision igesi ye-argon (> 99.999%). Ukushisa kwe-oven kuqale kusuka ku-80 ° C futhi kubanjelwe imizuzu eyi-1; kukhuphuke ngo-15 ° C / Min kuya ku-240 ° C, kwafika ku-260 ° C ku-20 ° C / min futhi ebanjwe nge-5min. Izinga lokushisa lomthombo we-ion lalingu-210 ° C, kanye nokushisa komugqa wokudlulisa kuka-280 ° C. I-the umjovo yevolumu yayingu-1.0 μl. Izimo ze-MRM zikhonjiswa kuThebula 3.

I-Agililent 8890 igesi i-chromatograph ifakwe nge-agililent 7000d kathathu quadrupole mass spectrometer (i-agilent, Stevens Creek, e-CA, USA) yayisetshenziselwa ukuhlaziya umphumela wokuhlanzwa nge-masshunter version 10.1 Software. Ikholomu ye-Agililent J & W HP-5MS GC (30 m × 0,25 mm × 0.25 μm) isetshenziselwe ukwehlukaniswa kwe-chromatomatic. I-Carrier Gream, i-Helium (> 99.999%), yahlelwa ngesilinganiso sokugeleza esingaguquki se-2.25 ml / min nge-collision igesi ye-nitrogen (> 99.999%). Izinga lokushisa lomthombo we-ei ion lalungiswa ku-280 ° C, okufanayo nokushisa komugqa wokudlulisa. Ukushisa kwe-oven kuqale kusuka ku-80 ° C futhi kwabanjwa imizuzu emi-5; Iphakanyiswe ngu-15 ° C / Min kuya ku-240 ° C, yabe isifinyelele kuma-280 ° C ku-25 ° C / min futhi yagcinwa imizuzu emi-5. Izimo ze-MRM zikhonjiswa kuThebula 3.

Ukuhlaziywa Kwezibalo
Okuqukethwe kwe-AQ emaqabungeni amasha kwalungiswa ukuze kususwe okuqukethwe kwendaba ngokuhlukanisa ngokuqukethwe komswakama ukuze uqhathanise futhi uhlaziye amazinga we-AQ ngesikhathi sokulungiswa.

Izinguquko ze-AQ kumasampula etiye zahlolwa nge-Microsoft Excel Software kanye ne-IBM SPSS Statistics 20.

I-Processing Factor yayisetshenziselwa ukuchaza izinguquko ku-AQ ngesikhathi sokucutshungulwa kwetiye. I-PF = RL / RF, lapho i-RF iyinqanaba le-AQ ngaphambi kokucubungula isinyathelo kanye ne-RL izinga le-AQ ngemuva kwesinyathelo sokucubungula. I-PF ikhombisa ukwehla (PF <1) noma ukwanda (PF> 1) ku-AQ okusele ngesikhathi sokucubungula okuthile.

Mina ngibonisa ukwehla (me <1) noma ukwanda (me> 1) Ukuphendula izinsimbi zokuhlaziya, ezisuselwa ku-ratios of matrix kanye ne-solvent kanje:

Me = (Slopematrix / Slopesolvent - 1) × 100%

Lapho i-slopematrix ingumbala we-calibration curve ku-solvent efaniswe ne-matrix, i-slopeslent yithambeka yokulinganisa ijika lokulinganisa ku-solvent.

Ukwamukela
Lo msebenzi wasekelwa yiprojekthi enkulu yesayensi nezobuchwepheshe esifundazweni saseZhejiang (2015c12001) kanye ne-National Science Foundation of China (42007354).
Ukungqubuzana Kwenzalo
Ababhali bathi abanakho ukungqubuzana kwenzalo.
Amalungelo nezimvume
I-copyright: © 2022 nguMlobi (s). Imali ekhethekile yelayisense yezemfundo yokufunda, i-fayetteville, ga. Le ndatshana iyisihloko sokufinyelela esivulekile esatshalaliswa ngaphansi kwelayisense ye-Creative Commons Attribution (CC ngo-4.0), vakashela ku-https: //creativecommons.org/censens/By/4.0/.
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