Abstract
I-9,10-Anthraquinone (AQ) iwukungcola okunobungozi obungaba yi-carcinogenic futhi yenzeka etiyeni emhlabeni wonke. Umkhawulo wensalela omkhulu (MRL) we-AQ etiyeni ebekwe yi-European Union (EU) ngu-0.02 mg/kg. Imithombo engaba khona ye-AQ ekucutshungulweni kwetiye kanye nezigaba eziyinhloko zokuvela kwayo kuye kwaphenywa ngokusekelwe endleleni yokuhlaziya ye-AQ elungisiwe kanye nokuhlaziywa kwe-gas chromatography-tandem mass spectrometry (GC-MS/MS). Uma kuqhathaniswa nogesi njengomthombo wokushisa ekucutshungulweni kwetiye eliluhlaza, i-AQ inyuke izikhathi ezingu-4.3 kuya kwezingu-23.9 ekucutshungulweni kwetiye ngamalahle njengomthombo wokushisa, edlula kude u-0.02 mg/kg, kuyilapho izinga le-AQ endaweni liphindaphindeka kathathu. Umkhuba ofanayo wabonwa ekucutshungulweni kwetiye le-oolong ngaphansi kokushisa kwamalahle. Izinyathelo ezinokuxhumana okuqondile phakathi kwamaqabunga etiye kanye nentuthu, njengokulungisa nokomisa, kubhekwa njengezinyathelo eziyinhloko zokukhiqizwa kwe-AQ ekucubunguleni itiye. Amazinga e-AQ anda ngokukhula kwesikhathi sokuxhumana, okuphakamisa ukuthi amazinga aphezulu e-AQ engcolisa itiye angase athathwe entumeni ebangelwa amalahle nokusha. Kwahlaziywa amasampula angamashumi amane avela kumaworkshop ahlukene anogesi noma amalahle njengemithombo yokushisa, asuka ku-50.0%−85.0% no-5.0%−35.0% ukuze atholwe futhi eqe amazinga e-AQ. Ukwengeza, okuqukethwe okuphezulu kwe-AQ okungu-0.064 mg/kg kubonwe emkhiqizweni wetiye namalahle njengomthombo wokushisa, okubonisa ukuthi amazinga aphezulu okungcola kwe-AQ emikhiqizweni yetiye kungenzeka anikele ngamalahle.
Amagama angukhiye: 9,10-Anthraquinone, Ukucubungula itiye, Amalahle, umthombo wokungcoliswa
ISINGENISO
Itiye elakhiwe ngamaqabunga esihlahla esihlala siluhlaza i-Camellia sinensis (L.) O. Kuntze, singesinye seziphuzo ezidume kakhulu emhlabeni wonke ngenxa yokunambitheka kwaso okuqabulayo kanye nezinzuzo zezempilo. Ngo-2020 emhlabeni jikelele, ukukhiqizwa kwetiye kukhuphuke kwafinyelela kumathani angama-metric ayizigidi ezingu-5,972, okwakuphindeke kabili eminyakeni engama-20 edlule[1]. Ngokusekelwe ezindleleni ezahlukene zokucubungula, kunezinhlobo eziyisithupha eziyinhloko zetiye, okuhlanganisa itiye eliluhlaza, itiye elimnyama, itiye elimnyama, itiye le-oolong, itiye elimhlophe kanye netiye eliphuzi[2,3]. Ukuqinisekisa ikhwalithi nokuphepha kwemikhiqizo, kubaluleke kakhulu ukuqapha amazinga okungcola nokuchaza umsuka.

Ukuhlonza imithombo yokungcola, njengezinsalela zezibulala-zinambuzane, izinsimbi ezisindayo nokunye ukungcola okufana ne-polycyclic aromatic hydrocarbons (PAHs), kuyisinyathelo esiyinhloko sokulawula ukungcola. Ukufuthwa okuqondile kwamakhemikhali okwenziwa emasimini etiye, kanye nokukhukhuleka komoya okubangelwa ukusebenza eduze nezingadi zetiye, kuwumthombo omkhulu wezinsalela zezibulala-zinambuzane etiyeni[4]. Izinsimbi ezinzima zinganqwabelana etiyeni futhi ziholele ebuthi, obutholakala ikakhulukazi enhlabathini, umanyolo kanye nomkhathi[5−7]. Ngokuqondene nokunye ukungcola okuvela kungazelelwe etiyeni, bekunzima kakhulu ukukubona ngenxa yezinqubo eziyinkimbinkimbi zochungechunge lokukhiqiza itiye okuhlanganisa ukutshala, ukucubungula, iphakheji, ukugcinwa kanye nokuhamba. Ama-PAH etiye avela ekufakweni kwezisi zezimoto kanye nokushiswa kwamafutha asetshenziswa ngesikhathi kucutshungulwa amaqabunga etiye, njengezinkuni namalahle[8−10].

Ngesikhathi sokusha kwamalahle nezinkuni, izinto ezingcolisayo njengama-carbon oxides ziyakhiwa[11]. Ngenxa yalokho, kungase kube lula ukuthi izinsalela zalokhu kungcola okukhulunywe ngenhla kwenzeke emikhiqizweni ecutshungulwayo, njengokusanhlamvu, izinhlanzi ezibhemayo kanye nezinhlanzi zekati, ekushiseni okuphezulu, okubeka usongo empilweni yomuntu[12,13]. Ama-PAH abangelwa ukusha asuselwa ekuguquguqukeni kwama-PAH aqukethwe kumafutha ngokwawo, ukubola kwezinga lokushisa eliphezulu kwezinhlanganisela ezinuka kamnandi kanye nokusabela okuyinhlanganisela phakathi kwama-radicals mahhala[14]. Izinga lokushisa lomlilo, isikhathi, nokuqukethwe komoyampilo yizici ezibalulekile ezithinta ukuguqulwa kwama-PAH. Ngokukhuphuka kwezinga lokushisa, okuqukethwe kwama-PAH kuqala kwanda kwase kwehla, futhi inani eliphakeme lenzeka ku-800 °C; Okuqukethwe kwama-PAH kwehle kakhulu ukuze kulandelelwe ngesikhathi esikhulayo sokuvutha lapho singaphansi komkhawulo obizwa ngokuthi 'isikhathi somngcele', nokwanda kokuqukethwe komoyampilo emoyeni ovuthayo, ukukhishwa kwe-PAHs kwehle kakhulu, kodwa i-oxidation engaphelele izokhiqiza ama-OPAH nokunye okuphuma kuyo[15] −17].

I-9,10-Anthraquinone (AQ, CAS: 84-65-1, Fig. 1), okuphuma komoya-mpilo okuphuma kuma-PAHs[18], iqukethe imijikelezo emithathu efingqiwe. Yafakwa kuhlu njenge-carcinogen engenzeka (Iqembu 2B) yi-International Agency for Research on Cancer ngo-2014[19]. I-AQ ingaba nobuthi ku-topoisomerase II cleavage complex futhi ivimbele i-hydrolysis ye-adenosine triphosphate (ATP) nge-DNA topoisomerase II, ibangele ukuphuka kwemicu ephindwe kabili ye-DNA, okusho ukuthi ukuchayeka isikhathi eside ngaphansi kwemvelo equkethe i-AQ kanye nokuxhumana okuqondile nezinga eliphezulu le-AQ. kungaholela ekulimaleni kwe-DNA, ukuguqulwa futhi kwandise ingozi yomdlavuza[20]. Njengemiphumela engemihle empilweni yomuntu, umkhawulo we-AQ maximum residue limit (MRL) ongu-0.02 mg/kg wabekwa etiyeni yi-European Union. Ngokwezifundo zethu zangaphambilini, idiphozithi ye-AQ yaphakanyiswa njengomthombo oyinhloko ngesikhathi sokutshala itiye[21]. Futhi, ngokusekelwe emiphumeleni yokuhlola ekucubunguleni itiye lase-Indonesia eliluhlaza nelimnyama, kusobala ukuthi izinga le-AQ lishintshe kakhulu futhi intuthu evela kumishini yokucubungula yaphakanyiswa njengenye yezizathu eziyinhloko[22]. Kodwa-ke, imvelaphi enembile ye-AQ ekucutshungulweni kwetiye yahlala ingaqondakali, nakuba ezinye izinkoleloze zendlela yamakhemikhali ye-AQ zaphakanyiswa [23,24], okubonisa ukuthi kubaluleke kakhulu ukucacisa izici ezibalulekile ezithinta izinga le-AQ ekucutshungulweni kwetiye.

Umfanekiso 1. Ifomula yamakhemikhali ye-AQ.

Njengoba kunikezwe ucwaningo ngokwakhiwa kwe-AQ ngesikhathi sokushiswa kwamalahle kanye nobungozi obungaba khona bamafutha ekucutshungulweni kwetiye, kwenziwa isilingo sokuqhathanisa ukuze kuchazwe umphumela wokucubungula imithombo yokushisa ku-AQ etiyeni nasemoyeni, ukuhlaziywa kwenani lokushintsha kokuqukethwe kwe-AQ. ezinyathelweni ezihlukene zokucubungula, okuwusizo ukuqinisekisa imvelaphi enembile, iphethini yokwenzeka kanye nezinga lokungcoliswa kwe-AQ ekucubunguleni itiye.

IMIPHUMELA
Ukuqinisekisa indlela
Uma kuqhathaniswa nocwaningo lwethu lwangaphambilini[21], inqubo yokukhipha uketshezi oluwuketshezi yahlanganiswa ngaphambi kokujova ku-GC-MS/MS ukuze kuthuthukiswe ukuzwela nokugcina izitatimende zamathuluzi. Ku-Fig 2b, indlela ethuthukisiwe ibonise ukuthuthukiswa okuphawulekayo ekuhlanzweni kwesampula, i-solvent yaba nombala okhanyayo. Ku-Fig 2a, i-spectrum egcwele yokuskena (50−350 m/z) ibonise ukuthi ngemva kokuhlanzwa, umugqa oyisisekelo we-MS spectrum uncishisiwe ngokusobala futhi iziqongo ezimbalwa ze-chromatographic zazitholakala, okubonisa ukuthi inani elikhulu lamakhompiyutha aphazamisayo asusiwe ngemva kokukhishwa kwe-chromatographic. ukukhishwa kwe-liquid-liquid.

Umfanekiso 2. (a) I-spectrum egcwele yokuskena yesampula ngaphambi nangemuva kokuhlanzwa. (b) Umthelela wokuhlanza wendlela ethuthukisiwe.
Ukuqinisekiswa kwendlela, okuhlanganisa umugqa, ukutholwa, umkhawulo we-quantitation (LOQ) kanye nomphumela we-matrix (ME), kuboniswa kuThebula 1. Kuyanelisa ukuthola umugqa one-coefficient of determination (r2) ephakeme kuno-0.998, esukela ku-0.005 ukuya ku-0.2 mg/kg ku-matrix yetiye ne-acetonitrile solvent, kanye nesampula yomoya enohlu lwe 0.5 kuya ku-8 μg/m3.

Ukutholwa kwe-AQ kwahlolwa ngokugxilisa okune-spiked okuthathu phakathi kokugxilisa okulinganiselwe kanye nokwangempela etiyeni elomile (0.005, 0.02, 0.05 mg/kg), amahlumela etiye amasha (0.005, 0.01, 0.02 mg/kg) kanye nesampula yomoya (0.5, 1.5, 3 μg/m3). Ukutholwa kwe-AQ etiyeni kusuka ku-77.78% kuya ku-113.02% etiyeni elomile futhi kusuka ku-96.52% kuya ku-125.69% emahlumela etiye, ne-RSD% engaphansi kuka-15%. Ukutholwa kwe-AQ kumasampula omoya kusukela ku-78.47% kuya ku-117.06% nge-RSD% engaphansi kuka-20%. I-concentration ene-spiked ephansi kakhulu ikhonjwe njenge-LOQ, okwakungu-0.005 mg/kg, 0.005 mg/kg kanye no-0.5 μg/m³ kumahlumela etiye, itiye elomile namasampula omoya, ngokulandelana. Njengoba kuboniswe kuThebula 1, i-matrix yetiye eyomile namahlumela etiye inyuse kancane impendulo ye-AQ, okuholela ku-ME ka-109.0% kanye no-110.9%. Mayelana ne-matrix yamasampula omoya, i-ME ibingu-196.1%.

Amazinga we-AQ ngesikhathi sokucubungula itiye elihlaza
Ngenhloso yokuthola imithelela yemithombo yokushisa ehlukene endaweni yetiye kanye nendawo yokucubungula, iqoqo lamaqabunga amasha lahlukaniswa laba amaqembu amabili akhethekile futhi acutshungulwa ngokwehlukana kumaworkshop amabili okucubungula ebhizinisini elifanayo. Iqembu elilodwa lalihlinzekwa ngogesi, elinye ngamalahle.

Njengoba kuboniswe ku-Fig. 3, izinga le-AQ elinogesi njengomthombo wokushisa lisukela ku-0.008 kuya ku-0.013 mg/kg. Ngesikhathi senqubo yokulungisa, ukubhakwa kwamaqabunga etiye okubangelwa ukugaywa ebhodweni elinokushisa okuphezulu kubangele ukwanda kwe-AQ ngo-9.5%. Khona-ke, izinga le-AQ lahlala ngesikhathi senqubo yokugoqa naphezu kokulahlekelwa ijusi, okusikisela ukuthi izinqubo zomzimba zingase zingathinti izinga le-AQ ekucubunguleni itiye. Ngemuva kwezinyathelo zokuqala zokumisa, izinga le-AQ lenyuke kancane lisuka ku-0.010 laya ku-0.012 mg/kg, labe seliqhubeka nokukhuphuka laya ku-0.013 mg/kg kuze kube sekupheleni kokumisa kabusha. Ama-PF, abonise ngokuphawulekayo ukuhluka esinyathelweni ngasinye, ayengu-1.10, 1.03, 1.24, 1.08 ekulungiseni, ekugingqeni, okokuqala omiswe futhi omiswe kabusha, ngokulandelanayo. Imiphumela yama-PFs iphakamise ukuthi ukucubungula ngaphansi kwamandla kagesi kube nomthelela omncane emazingeni e-AQ etiyeni.

Umfanekiso 3. Izinga le-AQ ngesikhathi sokucubungula itiye elihlaza ngogesi namalahle njengemithombo yokushisa.
Endabeni yamalahle njengomthombo wokushisa, okuqukethwe kwe-AQ kukhuphuke kakhulu ngesikhathi sokucubungula itiye, kusuka ku-0.008 kuya ku-0.038 mg/kg. I-338.9% AQ inyuswe kunqubo yokulungisa, yafinyelela ku-0.037 mg/kg, eyedlula kude i-MRL ka-0.02 mg/kg ebekwe yi-European Union. Ngesikhathi sokugingqika, izinga le-AQ lisakhuphuka ngo-5.8% naphezu kokuba kude nomshini wokulungisa. Ekomisweni kokuqala nasekumisweni kabusha, okuqukethwe kwe-AQ kwenyuke kancane noma kwehle kancane. Ama-PF asebenzisa amalahle njengomthombo wokushisa ekulungiseni, ukomisa kokuqala nokomisa kwakungu-4.39, 1.05, 0.93, kanye no-1.05, ngokulandelana.

Ukuze kuqhutshekwe kunqunywe ubudlelwano phakathi kokushiswa kwamalahle kanye nokungcoliswa kwe-AQ, izinto ezimisiwe (PMs) ezisemoyeni kuma-workshops ngaphansi kokubili kwemithombo yokushisa zaqoqwa ukuze kuhlolwe umoya, njengoba kukhonjisiwe kuFig. 4. Izinga le-AQ lama-PM anamalahle njenge umthombo wokushisa wawungu-2.98 μg/m3, owawungaphezu kokuphindwe kathathu kunogesi ongu-0.91 μg/m3.

Umfanekiso 4. Amazinga e-AQ endaweni enogesi namalahle njengomthombo wokushisa. * Ibonisa umehluko omkhulu kumazinga e-AQ kumasampuli (p <0.05).

Amazinga e-AQ ngesikhathi sokucubungula itiye le-Oolong, elikhiqizwa kakhulu e-Fujian nase-Taiwan, iwuhlobo lwetiye elivutshelwe kancane. Ukuze kuqhutshekwe nokunquma izinyathelo eziyinhloko zokukhulisa izinga le-AQ kanye nemithelela yezibaseli ezihlukene, iqoqo elifanayo lamaqabunga amasha lenziwe itiye le-oolong elinamalahle negesi yemvelo-ingxube kagesi njengemithombo yokushisa, ngesikhathi esisodwa. Amazinga e-AQ ekucutshungulweni kwetiye le-oolong kusetshenziswa imithombo yokushisa ehlukene aboniswa ku-Fig. 5. Ngokucubungula itiye le-oolong nge-hybrid gas-electric hybrid, ithrendi yeleveli ye-AQ ibilokhu imile ngaphansi kuka-0.005 mg/kg, eyayifana naleyo yetiye eliluhlaza. ngogesi.

Umfanekiso 5. Izinga le-AQ ngesikhathi sokucubungula itiye le-oolong ngengxube yegesi yemvelo kanye namalahle njengomthombo wokushisa.

Ngamalahle njengomthombo wokushisa, amaleveli e-AQ ezinyathelweni ezimbili zokuqala, abuna futhi enze luhlaza, ayefana ngokuyisisekelo nengxube yegesi yemvelo nogesi. Kodwa-ke, izinqubo ezalandela kuze kube yilapho ukulungiswa kukhombisa ukuthi igebe landa kancane kancane, lapho izinga le-AQ lenyuka lisuka ku-0.004 laya ku-0.023 mg/kg. Izinga esinyathelweni sokugoqa esigcwele lehlile laya ku-0.018 mg/kg, okungenzeka kungenxa yokulahlekelwa ijusi yetiye ethwala ezinye zezinto ezingcolisa i-AQ. Ngemuva kwesigaba sokugoqa, izinga esigabeni sokumisa lenyuke laya ku-0.027 mg/kg. Ekubuneni, ukwenza okuluhlaza, ukulungiswa, ukugoqa okupakishiwe nokomisa, ama-PF ayengu-2.81, 1.32, 5.66, 0.78, kanye no-1.50, ngokulandelana.

Ukuvela kwe-AQ emikhiqizweni yetiye enemithombo yokushisa ehlukene

Ukuze kutholakale imiphumela yokuqukethwe kwetiye kwe-AQ enemithombo yokushisa ehlukene, kwahlaziywa amasampula etiye angama-40 avela ezindaweni zokusebenzela zetiye esebenzisa ugesi noma amalahle njengemithombo yokushisa, njengoba kubonisiwe kuThebula 2. Uma kuqhathaniswa nokusebenzisa ugesi njengomthombo wokushisa, amalahle ayenawo kakhulu. amanani abaseshi (85.0%) anezinga eliphezulu le-AQ elingu-0.064 mg/kg, okubonisa ukuthi kwakulula ukubangela ukungcola kwe-AQ umusi okhiqizwa ukusha kwamalahle, kanye nezinga lama-35.0% labonwa kumasampula amalahle. Okugqame kakhulu, ugesi ubunezinga eliphansi labaphenyi kanye namazinga okusebenza ngokweqile angama-56.4% no-7.7% ngokulandelana, nokuqukethwe okuphezulu okungu-0.020 mg/kg.

INGXOXO

Ngokusekelwe kuma-PF ngesikhathi sokucutshungulwa ngezinhlobo ezimbili zemithombo yokushisa, kwacaca ukuthi ukulungiswa kwakuyisinyathelo esikhulu esaholela ekwandeni kwamazinga e-AQ ekukhiqizweni kwetiye ngamalahle nokucubungula ngaphansi kwamandla kagesi kube nomthelela omncane kokuqukethwe kwe-AQ. etiyeni. Ngesikhathi sokucutshungulwa kwetiye eliluhlaza, ukushiswa kwamalahle kwakhiqiza imfucumfucu eningi ohlelweni lokulungisa uma kuqhathaniswa nenqubo yokushisisa ngogesi, okubonisa ukuthi mhlawumbe intuthu yayiwumthombo oyinhloko wokungcola kwe-AQ ekuthinteni amahlumela etiye ngokushesha ekucutshungulweni kwetiye, okufana nenqubo yokuchayeka amasampula ezoso ezibhenywayo[25]. Ukwenyuka kancane kokuqukethwe kwe-AQ ngesikhathi sokugingqika kuphakamise ukuthi umusi obangelwa ukushiswa kwamalahle akuthinti kuphela ileveli ye-AQ phakathi nesinyathelo sokulungisa, kodwa futhi nasendaweni yokucubungula ngenxa yokumiswa komkhathi. Amalahle aphinde asetshenziswa njengomthombo wokushisa ekomisweni kokuqala nasekumisweni kabusha, kodwa kulezi zinyathelo ezimbili okuqukethwe kwe-AQ kunyuke kancane noma kwehle kancane. Lokhu kungase kuchazwe iqiniso lokuthi isomisi esinomoya oshisayo ebiyelwe sasigcina itiye kude nentuthu ebangelwa ukusha kwamalahle[26]. Ukuze kutholwe umthombo ongcolisayo, amazinga e-AQ emkhathini ahlaziywa, okubangele igebe elibalulekile phakathi kwama-workshops amabili. Isizathu esiyinhloko salokhu ukuthi amalahle asetshenziswa ekulungiseni, ezigabeni zokuqala zokomiswa nezomiswe kabusha azokhiqiza i-AQ ngesikhathi sokusha okungaphelele. Lawa ma-AQ abe esekhangiswa ezinhlayiyeni ezincane zezinto eziqinile ngemva kokusha kwamalahle futhi ahlakazeka emoyeni, aphakamisa amazinga okungcoliswa kwe-AQ endaweni yokusebenzela[15]. Ngokuhamba kwesikhathi, ngenxa yendawo enkulu ethize kanye namandla okukhangisa etiye, lezi zinhlayiya zibe sezihlala phezu kwamaqabunga etiye, okuholele ekwandeni kwe-AQ ekukhiqizeni. Ngakho-ke, ukushiswa kwamalahle kwakucatshangwa ukuthi kuyindlela eyinhloko eholela ekungcoleni kwe-AQ ngokweqile ekucubungulweni kwetiye, nentuthu iwumthombo wokungcola.

Ngokuqondene nokucutshungulwa kwetiye le-oolong, i-AQ inyuswe ngaphansi kokucubungula ngayo yomibili imithombo yokushisa, kodwa umehluko phakathi kwemithombo yokushisa emibili wawubalulekile. Imiphumela iphinde yaphakamisa ukuthi amalahle njengomthombo wokushisa adlale indima enkulu ekwandiseni izinga le-AQ, futhi ukulungiswa kwathathwa njengesinyathelo esiyinhloko sokwandisa ukungcoliswa kwe-AQ ekucubunguleni itiye le-oolong ngokusekelwe kuma-PF. Ngesikhathi sokucutshungulwa kwetiye le-oolong nge-hybrid gas-electric hybrid njengomthombo wokushisa, ukuthambekela kwezinga le-AQ kwakumile ngaphansi kuka-0.005 mg/kg, okwakufana naleyo yetiye eliluhlaza elinogesi, okuphakamisa ukuthi amandla ahlanzekile, njengogesi nemvelo. igesi, inganciphisa ubungozi bokukhiqiza ukungcola kwe-AQ kusukela ekucutshungulweni.

Mayelana nokuhlolwa kwamasampula, imiphumela yabonisa ukuthi isimo sokungcoliswa kwe-AQ sasibi kakhulu uma kusetshenziswa amalahle njengomthombo wokushisa kunogesi, okungase kubangelwe yintuthu yokushiswa kwamalahle ehlangana namahlamvu etiye nokuzulazula endaweni yokusebenza. Nokho, nakuba kwakusobala ukuthi ugesi wawuwumthombo wokushisa ohlanzekile phakathi nokucubungula itiye, kwakusenokungcola kwe-AQ emikhiqizweni yetiye esebenzisa ugesi njengomthombo wokushisa. Isimo sibonakala sifana kancane nomsebenzi oshicilelwe ngaphambilini lapho ukusabela kwe-2-alkenals nama-hydroquinones nama-benzoquinones kwaphakanyiswa njengendlela engase ibe yindlela yamakhemikhali[23], izizathu zalokhu zizophenywa ocwaningweni oluzayo.

IZIPHETHO

Kulo msebenzi, imithombo engaba khona yokungcoliswa kwe-AQ etiyeni eliluhlaza kanye ne-oolong yaqinisekiswa ukuhlola okuqhathanisayo okusekelwe ezindleleni zokuhlaziya ze-GC-MS/MS ezithuthukisiwe. Okutholwe kwethu kusekela ngokuqondile ukuthi umthombo oyinhloko ongcolisayo wamazinga aphezulu e-AQ kwakuwumusi obangelwa ukusha, okungagcini nje ngokuthinta izigaba zokucubungula kodwa futhi kuthinte indawo yokusebenzela. Ngokungafani nezigaba zokugoqa nokubuna, lapho izinguquko ezingeni le-AQ zazingabonakali, izigaba ngokubandakanyeka okuqondile kwamalahle nezinkuni, njengokulungiswa, inqubo eyinhloko lapho ukungcoliswa kwe-AQ kukhuphuke ngenxa yenani lokuxhumana phakathi kwetiye. kanye nentuthu phakathi nalezi zigaba. Ngakho-ke, amafutha ahlanzekile afana negesi yemvelo nogesi kwanconywa njengomthombo wokushisa ekucubunguleni itiye. Ukwengeza, imiphumela yokuhlola iphinde yabonisa ukuthi ngenxa yokungabikho kwentuthu ekhiqizwa ukusha, kwakusenezinye izici ezinomthelela ekulandeleni i-AQ ngesikhathi sokucubungula itiye, kuyilapho amanani amancane e-AQ abuye abonwa ku-workshop esebenzisa amafutha ahlanzekile, okufanele aphenywe. ocwaningweni oluzayo.

IZIMPAHLA NEZINDLELA

Ama-reagents, amakhemikhali nezinto zokwakha

Izinga le-anthraquinone (99.0%) lathengwa ku-Dr. Ehrenstorfer GmbH Company (Augsburg, Germany). Izinga langaphakathi le-D8-Anthraquinone (98.6%) lathengwa kwa-C/D/N Isotopes (Quebec, Canada). I-Anhydrous sodium sulfate (Na2SO4) ne-magnesium sulfate (MgSO4) (Shanghai, China). I-Florisil yahlinzekwa yi-Wenzhou Organic Chemical Company (Wenzhou, China). Iphepha le-Mircro-glass fiber (90 mm) lathengwa enkampanini i-Ahlstrom-munksjö (Helsinki, Finland).

Ukulungiselela isampula

Amasampula etiye elihlaza acutshungulwa ngokulungiswa, ukugoqwa, omiswe kuqala futhi omiswe kabusha (kusetshenziswa impahla evalekile), kuyilapho amasampula etiye e-oolong acutshungulwa ngokubuna, enze aluhlaza (amahlamvu anyakazayo nokuma amasha ngokushintshana), ukulungiswa, ukugoqa okupakishiwe, kanye ukomisa. Amasampula asuka esinyathelweni ngasinye aqoqwa kathathu ku-100g ngemva kokuxubana okuphelele. Wonke amasampula agcinwe ku-−20 °C ukuze aqhubeke nokuhlaziywa.

Amasampula omoya aqoqwe ngephepha le-glass fiber (90 mm) kusetshenziswa amasampula evolumu ephakathi (PTS-100, Qingdao Laoshan Electronic Instrument Company, Qingdao, China)[27], asebenza ku-100 L/min amahora angu-4.

Amasampula aqinisiwe afakwe nge-AQ ku-0.005 mg/kg, 0.010 mg/kg, 0.020 mg/kg amahlumela etiye amasha, ku-0.005 mg/kg, 0.020 mg/kg, 0.050 mg/kg wetiye elomile futhi ku-0.012 mg/kg (0.5 µg/m3 ngesampula yomoya), 0.036 mg/kg (1.5 µg/m3 ye-air smaple), 0.072 mg/kg (3.0 µg/m3 yesampula yomoya) wephepha lesihlungi sengilazi, ngokulandelanayo. Ngemuva kokugubha kahle, wonke amasampula ashiywe amahora angu-12, alandelwe izinyathelo zokukhipha kanye nokuhlanza.

Okuqukethwe komswakamo kutholwe ngokuthatha u-20 g wesampula ngemva kokuxuba isinyathelo ngasinye, ukushisisa ku-105 °C ihora elingu-1, bese kukala futhi kuphindwe kathathu futhi kuthathwe inani elimaphakathi futhi kulihlukanise ngesisindo ngaphambi kokushisisa.

Ukukhishwa kwesampula nokuhlanza

Isampula yetiye: Ukukhishwa nokuhlanzwa kwe-AQ kumasampula etiye kwenziwa ngokusekelwe endleleni eshicilelwe evela ku-Wang et al. nezimo eziningana [21]. Kafushane, u-1.5 g wamasampula etiye aqale axutshwa no-30 μL D8-AQ (2 mg/kg) futhi ayekwa ukuthi ame imizuzu engama-30, abese exutshwa kahle no-1.5 mL amanzi akhiqiziwe futhi ayekwe ukuze ame imizuzu engama-30. I-15 mL 20% i-acetone ku-n-hexane yengezwe kumasampula etiye futhi yafakwa i-sonicated imizuzu eyi-15. Khona-ke amasampula avuthwa nge-1.0 g MgSO4 ye-30 s, futhi agxilwe phakathi kwamaminithi angu-5, ngo-11,000 rpm. Ngemva kokuthuthelwa kumaflask angu-100 ml amise okwepheya, u-10 mL wesigaba sezinto eziphilayo wahwamuka wacishe woma ngaphansi kwe-vacuum engu-37 °C. 5 mL 2.5% i-acetone ku-n-hexane iphinde yancibilikisa i-extract kumaflask amise okwepheya ukuze ihlanzwe. Ikholomu yengilazi (10 cm × 0.8 cm) yayihlanganisa kusukela phansi kuya phezulu koboya bengilazi kanye no-2g florisil, owawuphakathi kwezingqimba ezimbili ze-2 cm Na2SO4. Bese u-5 mL ka-2.5% we-acetone ku-n-hexane egeza kuqala ikholomu. Ngemva kokulayisha isixazululo esihlakazeke kabusha, i-AQ yakhishwa izikhathi ezintathu ngo-5 mL, 10 mL, 10 mL we-acetone engu-2.5% ku-n-hexane. Ama-eluate ahlanganisiwe adluliselwa kumaflask amise okwepheya futhi ahwamuke acishe ome ngaphansi kwe-vacuum engu-37 °C. Izinsalela ezomisiwe zibe sezihlanganiswa kabusha nge-1 mL ye-acetone engu-2.5% ku-hexane elandelwa ukuhlungwa ngesihlungi sosayizi wezimbotshana esingu-0.22 µm. Khona-ke isixazululo esilungisiwe sihlanganiswe ne-acetonitrile ngesilinganiso somthamo we-1: 1. Ngokulandela isinyathelo esinyakazayo, i-subnatant yasetshenziselwa ukuhlaziya i-GC-MS/MS.

Isampula yomoya: Uhhafu wephepha le-fiber, eliconsiswe nge-18 μL d8-AQ (2 mg/kg), lacwiliswa ku-15 mL we-20% i-acetone ku-n-hexane, yase ifakwa i-sonication imizuzu engu-15. Isigaba sezinto eziphilayo sahlukaniswa nge-centrifugation ku-11,000 rpm imizuzu engu-5 futhi lonke ungqimba olungaphezulu lwasuswa ku-flask emise okwepheya. Zonke izigaba zemvelo zahwamuka zacishe zoma ngaphansi kwe-vacuum engu-37 °C. I-5 mL ka-2.5% i-acetone ku-hexane incibilikise kabusha okukhishwe ukuze kuhlanzwe ngendlela efanayo namasampula etiye.

Ukuhlaziywa kwe-GC-MS/MS

I-Varian 450 gas chromatograph efakwe i-Varian 300 tandem mass detector (Varian, Walnut Creek, CA, USA) yasetshenziswa ukwenza ukuhlaziya kwe-AQ ngesofthiwe ye-MS WorkStation engu-6.9.3. I-Varian Factor Ikholomu ye-capillary Four VF-5ms (30 m × 0.25 mm × 0.25 μm) yasetshenziselwa ukuhlukaniswa kwe-chromatographic. Igesi yenkampani yenethiwekhi, i-helium (> 99.999%), isethwe kuzinga lokugeleza elingaguquki elingu-1.0 mL/min negesi yokushayisana ye-Argon (> 99.999%). Izinga lokushisa likahhavini liqale ukusuka ku-80 °C futhi libambe iminithi elingu-1; inyuke ngo-15 °C/min kuya ku-240 °C, bese ifinyelela ku-260 °C ku-20 °C/min futhi ibanjwe imizuzu engu-5. Izinga lokushisa lomthombo we-ion lalingu-210 °C, kanye nezinga lokushisa lomugqa wokudlulisa elingu-280 °C. Umthamo womjovo wawuyi-1.0 μL. Izimo ze-MRM zivezwe kuThebula lesi-3.

I-Agilent 8890 gas chromatograph ifakwe i-Agilent 7000D triple quadrupole mass spectrometer (Agilent, Stevens Creek, CA, USA) yasetshenziswa ukuhlaziya umphumela wokuhlanza ngesoftware ye-MassHunter 10.1. I-Agilent J&W HP-5ms GC Ikholomu (30 m × 0.25 mm × 0.25 μm) isetshenziselwe ukuhlukaniswa kwe-chromatographic. Igesi elithwala impahla, i-Helium (> 99.999%), ibekwe ezingeni lokugeleza elingaguquki elingu-2.25 mL/min negesi yokushayisana ye-Nitrogen (> 99.999%). Izinga lokushisa lomthombo we-ion we-EI lilungiswe ku-280 °C, ngokufanayo nezinga lokushisa lomugqa wokudlulisa. Izinga lokushisa likahhavini liqale ukusuka ku-80 °C futhi libanjwe imizuzu emi-5; inyuswe ngo-15 °C/min kuya ku-240 °C, bese ifinyelela ku-280 °C ku-25 °C/min futhi igcinwe imizuzu emi-5. Izimo ze-MRM zivezwe kuThebula lesi-3.

Ukuhlaziywa kwezibalo
Okuqukethwe kwe-AQ emaqabunga amasha kwalungiswa ukuze kome okuqukethwe ngokuhlukaniswa ngokuqukethwe komswakama ukuze kuqhathaniswe futhi kuhlaziywe amaleveli e-AQ phakathi nokucubungula.

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

Isici sokucubungula sisetshenziswe ukuchaza izinguquko ku-AQ ngesikhathi sokucubungula itiye. PF = Rl/Rf , lapho i-Rf iyileveli ye-AQ ngaphambi kwesinyathelo sokucubungula futhi i-Rl iyizinga le-AQ ngemva kwesinyathelo sokucubungula. I-PF ikhombisa ukwehla (PF <1) noma ukwenyuka (PF > 1) kwensalela ye-AQ phakathi nesinyathelo sokucubungula esithile.

I-ME ikhombisa ukwehla (ME < 1) noma ukunyuka (ME > 1) ekuphenduleni kumathuluzi okuhlaziya, okusekelwe esilinganisweni semithambeka yokulinganiswa ku-matrix ne-solvent kanje:

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

Lapho i-slopematrix iwumthambeka wejika lokulinganisa ku-solvent efana ne-matrix, i-slopesolvent iwumthambeka wejika lokulinganisa ku-solvent.

AMABONGWA
Lo msebenzi usekelwe iSayensi Nobuchwepheshe Iphrojekthi Enkulu esifundazweni saseZhejiang (2015C12001) kanye neNational Science Foundation yaseChina (42007354).
Ukungqubuzana kwezintshisekelo
Ababhali bamemezela ukuthi abanakho ukungqubuzana kwezintshisekelo.
Amalungelo nezimvume
I-Copyright: © 2022 yombhali(ababhali). I-Exclusive Licensee Maximum Academic Press, Fayetteville, GA. Lesi sihloko siyi-athikili yokufinyelela evulekile esatshalaliswa ngaphansi kwe-Creative Commons Attribution License (CC BY 4.0), vakashela ku-https://creativecommons.org/licenses/by/4.0/.
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