Abstract
I-9,10-Anthraquinone (AQ) yinto engcolileyo enokuthi ibe yingozi ye-carcinogenic kwaye iyenzeka kwiti emhlabeni jikelele.Ubuninzi bomda wentsalela (MRL) ye-AQ kwiti esetwe yi-European Union (EU) yi-0.02 mg/kg.Imithombo enokubakho ye-AQ ekuqhutyweni kweti kunye nezigaba eziphambili zokuvela kwayo ziphandwe ngokusekelwe kwindlela yohlalutyo ye-AQ elungisiweyo kunye ne-gas chromatography-tandem mass spectrometry (GC-MS / MS) uhlalutyo.Xa kuthelekiswa nombane njengomthombo wobushushu ekusetyenzweni kweti eluhlaza, i-AQ inyuke ngama-4.3 ukuya kuma-23.9 ngamaxesha ekusetyenzweni kweti ngamalahle njengomthombo wobushushu, idlula kakhulu i-0.02 mg/kg, ngelixa inqanaba le-AQ kwimekobume liphindwe kathathu.Umkhwa ofanayo wabonwa ekusetyenzweni kweti ye-oolong phantsi kobushushu bamalahle.Amanyathelo anokuqhagamshelana ngokuthe ngqo phakathi kwamagqabi eti kunye nomphunga, njengokulungiswa kunye nokomisa, kuthathwa njengamanyathelo aphambili emveliso ye-AQ ekuqhutyweni kwetiyi.Amanqanaba e-AQ anda ngokunyuka kwexesha loqhagamshelwano, ebonisa ukuba amanqanaba aphezulu e-AQ engcolisa iti anokuthi athathwe kwi-fumes ebangelwa ngamalahle kunye nokutsha.Iisampulu ezingamashumi amane ezivela kwiindibano zocweyo ezahlukeneyo ezinombane okanye amalahle njengemithombo yobushushu zahlalutywa, ukusuka kwi-50.0% -85.0% kunye ne-5.0% -35.0% yokufunyanwa kunye nokugqithiswa kweereyithi ze-AQ.Ukongezelela, umxholo we-AQ ophezulu we-0.064 mg / kg wabonwa kwimveliso yeti kunye namalahle njengomthombo wokushisa, ebonisa ukuba amanqanaba aphezulu okungcola kwe-AQ kwiimveliso zeti kunokwenzeka ukuba afakwe ngamalahle.
Amagama angundoqo: i-9,10-Anthraquinone, iTea processing, amalahle, umthombo wokuNgcola
INTSHAYELELO
Iti eyenziwe ngamagqabi esihlahla esihlala siluhlaza iCamellia sinensis (L.) O. Kuntze, sesinye seziselo ezidumileyo kwihlabathi ngenxa yencasa yaso ehlaziyayo kunye neenzuzo zempilo.Ngo-2020 kwihlabathi jikelele, imveliso yeti yonyuke yaya kutsho kwi-5,972 yezigidi zeetoni zeemetric, nto leyo ibiphindaphindeka kule minyaka ingama-20 idlulileyo[1].Ngokusekwe kwiindlela ezahlukeneyo zokusetyenzwa, kukho iintlobo ezintandathu eziphambili zeti, ezibandakanya iti eluhlaza, iti emnyama, iti emnyama, i-oolong, iti emhlophe kunye neti emthubi[2,3].Ukuqinisekisa umgangatho kunye nokhuseleko lweemveliso, kubaluleke kakhulu ukubeka iliso kumanqanaba okungcola kunye nokuchaza imvelaphi.

Ukuchonga imithombo yongcoliseko, njengeentsalela zezibulali-zinambuzane, isinyithi esinzima kunye nezinye izinto ezingcolisayo ezifana ne-polycyclic aromatic hydrocarbons (PAHs), linyathelo eliphambili lokulawula ungcoliseko.Ukutshizwa ngokuthe ngqo kweekhemikhali zokwenziwa kumasimi eti, kunye nokuqhutywa komoya okubangelwa yimisebenzi ekufutshane nezitiya zeti, ngowona mthombo weentsalela zezitshabalalisi kwiti[4].Iintsimbi ezinzima zinokuqokelelana kwiti kwaye zikhokelela kwityhefu, ephuma ikakhulu kumhlaba, isichumisi kunye nomoya[5-7].Ngokumalunga nolunye ungcoliseko oluvela ngokungalindelekanga etini, kwakunzima kakhulu ukuchonga ngenxa yeenkqubo ezintsonkothileyo zekhonkco lemveliso yeti ezibandakanya ukutyalwa, ukusetyenzwa, ukupakishwa, ukugcinwa kunye nokuthutha.I-PAHs kwiti yavela ekubekweni kombhobho wezithuthi kunye nokutshiswa kwamafutha asetyenziswa ngexesha lokulungiswa kwamagqabi eti, njengeenkuni kunye namalahle[8-10].

Ngexesha lokutsha kwamalahle neenkuni, ungcoliseko olufana necarbon oxides luyakheka[11].Ngenxa yoko, kuyenzeka ukuba iintsalela zezi zinto zingcolileyo zikhankanywe ngasentla zenzeke kwiimveliso ezicutshungulwayo, ezifana nengqolowa, i-stocks smoked fish kunye nentlanzi yekati, kwiqondo lokushisa eliphezulu, elibeka ingozi kwimpilo yabantu [12,13].I-PAHs ezibangelwa kukutsha zisuka ku-volatilization ye-PAHs eziqulethwe kumafutha ngokwawo, ukubola okuphakamileyo kobushushu bezinto ezivumbayo kunye nempendulo edibeneyo phakathi kweeradicals zamahhala[14].Ukushisa okutshisayo, ixesha, kunye nomxholo we-oksijini zizinto ezibalulekileyo ezichaphazela ukuguqulwa kwee-PAHs.Ngokunyuka kweqondo lokushisa, umxholo we-PAHs waqala ukwanda kwaye wehla, kwaye ixabiso eliphezulu lenzeke kwi-800 ° C;Umxholo we-PAHs wehla ngokukhawuleza ukulandelela ngokunyuka kwexesha lokutshisa xa lingaphantsi komda obizwa ngokuba 'ixesha lomda', ngokunyuka komxholo we-oksijini emoyeni ovuthayo, ukukhutshwa kwe-PAHs kuncitshiswe kakhulu, kodwa i-oxidation engaphelelanga iya kuvelisa i-OPAHs kunye nezinye izinto eziphumayo [15] −17].

I-9,10-Anthraquinone (AQ, CAS: 84-65-1, Umfanekiso 1), i-oksijini ephuma kwi-PAHs [18], iqulethwe imijikelezo emithathu edibeneyo.Yayidweliswe njenge-carcinogen enokwenzeka (iQela le-2B) yi-Arhente yamazwe ngamazwe yoPhando lweCancer kwi-2014 [19].I-AQ inokutyhefa kwi-topoisomerase II cleavage complex kwaye inqanda i-hydrolysis ye-adenosine triphosphate (ATP) nge-DNA topoisomerase II, ibangela i-DNA ikhefu eliphindwe kabini, oku kuthetha ukuba ukuvezwa kwexesha elide phantsi kwe-AQ-equlethe indawo kunye noqhagamshelwano oluthe ngqo kunye nenqanaba eliphezulu le-AQ. kunokukhokelela kumonakalo we-DNA, ukuguqulwa kunye nokwandisa ingozi yomhlaza[20].Njengeempembelelo ezimbi kwimpilo yabantu, i-AQ i-residue limit limit (MRL) ye-0.02 mg / kg ibekwe kwiti yi-European Union.Ngokwezifundo zethu zangaphambili, iidiphozithi ze-AQ zacetyiswa njengowona mthombo uphambili ngexesha lokulima iti[21].Kwakhona, ngokusekelwe kwiziphumo zovavanyo kwi-Indonesian eluhlaza kunye ne-black tea processing, kuyacaca ukuba inqanaba le-AQ litshintshe kakhulu kwaye umsi ovela kwizixhobo zokusebenza wacetyiswa njengenye yezizathu eziphambili[22].Nangona kunjalo, imvelaphi echanekileyo ye-AQ ekusebenzeni kweti yahlala ingenakwenzeka, nangona ezinye iingcamango ze-AQ zendlela yeekhemikhali zacetyiswa [23,24], ebonisa ukuba kubaluleke kakhulu ukufumanisa izinto ezibalulekileyo ezichaphazela inqanaba le-AQ ekusetyenzweni kweti.

Umzobo 1. Ifomula yekhemikhali ye-AQ.

Ukunikezelwa kophando malunga nokusekwa kwe-AQ ngexesha lokutsha kwamalahle kunye nobungozi obunokubakho bamafutha ekusebenzeni kweti, uvavanyo lokuthelekisa lwenziwa ukucacisa isiphumo sokusetyenzwa kwemithombo yobushushu kwi-AQ kwiti kunye nomoya, uhlalutyo lobungakanani kwiinguqu zomxholo we-AQ. kumanyathelo okusebenza ahlukeneyo, aluncedo ekuqinisekiseni imvelaphi echanekileyo, ipateni yokwenzeka kunye neqondo longcoliseko lwe-AQ ekusetyenzweni kweti.

IZIPHUMO
Indlela yokuqinisekisa
Xa kuthelekiswa nesifundo sethu sangaphambili [21], inkqubo yokukhutshwa kwe-liquid-liquid yadityaniswa ngaphambi kokuba inaliti kwi-GC-MS / MS ukwenzela ukuphucula ubuntununtunu kunye nokugcina iingxelo zezixhobo.Kwi-Fig 2b, indlela ephuculweyo ibonise ukuphucuka okubalulekileyo ekuhlanjululweni kwesampuli, i-solvent yaba yinto elula ngombala.Kwi-Fig 2a, i-scan scan spectrum (50-350 m / z) ibonise ukuba emva kokuhlanjululwa, umgca wesiseko we-MS spectrum wanciphisa ngokucacileyo kwaye iinqununu ezimbalwa ze-chromatographic zikhoyo, ezibonisa ukuba inani elikhulu lezinto eziphazamisayo zisuswe emva kokuba ukutsalwa kolwelo.

Umzobo 2. (a) I-spectrum epheleleyo yokuskena isampuli ngaphambi nangemva kokucoca.(b) Isiphumo sokucoca sendlela ephuculweyo.
Indlela yokuqinisekisa, kubandakanywa umgca, ukubuyiswa, umda we-quantitation (LOQ) kunye ne-matrix effect (ME), iboniswe kwiThebhile 1. Kuyanelisa ukufumana umgca kunye ne-coefficient of determination (r2) ephezulu kune-0.998, ephuma kwi-0.005 ukuya kwi-0.2 mg / kg kwi-tea matrix kunye ne-acetonitrile solvent, kunye nesampuli yomoya kunye noluhlu lwe-0.5 ukuya kwi-8 μg / m3.

Ukubuyiswa kwe-AQ kwavavanywa kwiinkalo ezintathu ze-spiked phakathi kokulinganisa kunye nokugxininiswa kwangempela kwiti eyomileyo (0.005, 0.02, 0.05 mg / kg), i-tea shoots fresh (0.005, 0.01, 0.02 mg / kg) kunye nesampuli yomoya (0.5, 1.5, 3 μg/m3).Ukubuyiswa kwe-AQ kwiti ukusuka kwi-77.78% ukuya kwi-113.02% kwiti eyomileyo kwaye ukusuka kwi-96.52% ukuya kwi-125.69% kwi-tea shoots, kunye ne-RSD engaphantsi kwe-15%.Ukubuyiswa kwe-AQ kwiisampuli zomoya ukusuka kwi-78.47% ukuya kwi-117.06% kunye ne-RSD% ngaphantsi kwe-20%.Olona gxininiso lwe-spiked lusezantsi lwachongwa njenge-LOQ, eyayiyi-0.005 mg/kg, 0.005 mg/kg kunye ne-0.5 μg/m³ kumahlumelo eti, iti eyomileyo kunye neesampuli zomoya, ngokulandelelanayo.Njengoko kudweliswe kwiThebhile 1, i-matrix yeti eyomileyo kunye ne-tea shoots yandisa kancinci impendulo ye-AQ, ekhokelela kwi-ME ye-109.0% kunye ne-110.9%.Ngokumalunga ne-matrix yeesampulu zomoya, i-ME yayiyi-196.1%.

Amanqanaba e-AQ ngexesha lokucubungula iti eluhlaza
Ngenjongo yokufumanisa iziphumo zemithombo eyahlukeneyo yobushushu kwimo yeti kunye nokusetyenzwa kwayo, ibhetshi yamagqabi amatsha yahlulwa yangamaqela amabini athile kwaye yalungiswa ngokwahlukeneyo kwiindibano zocweyo ezimbini zokusetyenzwa kwishishini elinye.Elinye iqela labonelelwa ngombane, elinye ngamalahle.

Njengoko kuboniswe kwi-Fig. 3, inqanaba le-AQ ngombane njengomthombo wokushisa ukusuka kwi-0.008 ukuya kwi-0.013 mg / kg.Ngethuba lenkqubo yokulungisa, ukutshisa kwamagqabi eti okubangelwa ukucutshungulwa embizeni enobushushu obuphezulu kubangele ukunyuka kwe-9.5% kwi-AQ.Emva koko, inqanaba le-AQ lahlala ngexesha lenkqubo yokuqengqeleka nangona ilahleko yejusi, ebonisa ukuba iinkqubo zomzimba zingenako ukuchaphazela inqanaba le-AQ ekusebenzeni kweti.Emva kwamanyathelo okuqala okumisa, inqanaba le-AQ landa kancane ukusuka kwi-0.010 ukuya kwi-0.012 mg / kg, emva koko yaqhubeka inyuka ukuya kwi-0.013 mg / kg de kube sekupheleni kokumisa kwakhona.I-PFs, ebonisa ngokuphawulekayo ukuhluka kwinqanaba ngalinye, yayiyi-1.10, 1.03, 1.24, 1.08 ekulungiseni, ukugoqa, ukumisa okokuqala kunye nokumisa kwakhona, ngokulandelanayo.Iziphumo zePFs zicebise ukuba ukucubungula phantsi kwamandla ombane kunempembelelo encinci kumanqanaba e-AQ kwiti.

Umzobo 3. Inqanaba le-AQ ngexesha lokucubungula iti eluhlaza ngombane kunye namalahle njengemithombo yokushisa.
Kwimeko yamalahle njengomthombo wokushisa, umxholo we-AQ unyuke ngokukhawuleza ngexesha lokucubungula iti, ukunyuka ukusuka kwi-0.008 ukuya kwi-0.038 mg / kg.I-338.9% ye-AQ yonyuswa kwinkqubo yokulungisa, ifikelela kwi-0.037 mg / kg, egqithise kakhulu i-MRL ye-0.02 mg / kg ebekwe yi-European Union.Ngexesha lokuqengqeleka, inqanaba le-AQ lisanyuka nge-5.8% nangona likude kumatshini wokulungisa.Ekomisweni kokuqala kunye nokumisa kwakhona, umxholo we-AQ wanda kancinci okanye wehla kancinci.I-PFs isebenzisa amalahle njengomthombo wokushisa ekulungiseni, ukuqengqeleka kokuqala kunye nokumisa kwakhona kwakuyi-4.39, 1.05, 0.93, kunye ne-1.05, ngokulandelanayo.

Ukuqinisekisa ngakumbi ubudlelwane phakathi kokutsha kwamalahle kunye nongcoliseko lwe-AQ, imiba ye-particulate emisiweyo (PMs) emoyeni kwiindibano zocweyo phantsi kwemithombo yomibini yobushushu yaqokelelwa kuvavanyo lomoya, njengoko kubonisiwe kumfanekiso 4. Inqanaba le-AQ le-PMs ngamalahle njengamalahle njenge umthombo wokushisa wawuyi-2.98 μg / m3, eyayingaphezulu ngokuphindwe kathathu kunombane 0.91 μg / m3.

Umzobo 4. Amanqanaba e-AQ kwindawo enombane kunye namalahle njengomthombo wobushushu.* Ibonisa ukungafani okuphawulekayo kumanqanaba e-AQ kwiisampuli (p <0.05).

Amanqanaba e-AQ ngexesha leti ye-oolong yokusetyenzwa kweti i-Oolong, eveliswa ikakhulu eFujian naseTaiwan, luhlobo lweti enegwele ngokuyinxenye.Ukucacisa ngakumbi amanyathelo aphambili okunyusa inqanaba le-AQ kunye nemiphumo yamafutha ahlukeneyo, ibhetshi efanayo yamagqabi amatsha yenziwe iti ye-oolong kunye namalahle kunye negesi yendalo-yombane we-hybrid njengemithombo yokushisa, ngaxeshanye.Amanqanaba e-AQ ekusetyenzweni kweti ye-oolo usebenzisa imithombo yobushushu eyahlukeneyo iboniswe kwi-Fig. 5. Ukulungiselela iti ye-oolong kunye ne-hybrid yegesi yendalo yombane, umgangatho we-AQ wawudodobala ngaphantsi kwe-0.005 mg / kg, eyayifana naleyo kwiti eluhlaza. ngombane.

Umzobo 5. Inqanaba le-AQ ngexesha lokucutshungulwa kweti ye-oolong kunye ne-natural gas-electric blend kunye namalahle njengomthombo wobushushu.

Ngamalahle njengomthombo wobushushu, amanqanaba e-AQ kumanyathelo amabini okuqala, ukubuna kunye nokwenza uhlaza, ayefana ngokusisiseko nomxube wegesi yendalo yombane.Nangona kunjalo, iinkqubo ezilandelayo de ukulungiswa kwabonisa ukuba i-gap yanda ngokuthe ngcembe, apho inqanaba le-AQ linyuka ukusuka kwi-0.004 ukuya kwi-0.023 mg / kg.Inqanaba kwinqanaba lokupakisha lehla ukuya kwi-0.018 mg / kg, enokuthi ibe ngenxa yokulahlekelwa kwejusi yeti ethwele ezinye ze-AQ ezingcolileyo.Emva kwesigaba sokuqengqeleka, izinga kwinqanaba lokumisa liye landa kwi-0.027 mg / kg.Ekubuneni, ukwenza uhlaza, ukulungiswa, ukupakisha ukupakisha kunye nokomisa, i-PFs yayiyi-2.81, 1.32, 5.66, 0.78, kunye ne-1.50, ngokulandelanayo.

Ukwenzeka kwe-AQ kwiimveliso zeti ezinemithombo eyahlukeneyo yobushushu

Ukumisela iziphumo kumxholo we-AQ weti enemithombo eyahlukeneyo yobushushu, iisampulu zeti ezingama-40 ezivela kwiindibano zocweyo zisebenzisa umbane okanye amalahle njengemithombo yobushushu yahlalutywa, njengoko kubonisiwe kwiThebhile 2. Xa kuthelekiswa nokusebenzisa umbane njengomthombo wobushushu, amalahle ayenawona maninzi. amazinga omcuphi (85.0%) kunye nenqanaba eliphezulu le-AQ ye-0.064 mg / kg, ebonisa ukuba kwakulula ukwenza i-AQ ingcoliseke yimfucu eveliswa ngokutshiswa kwamalahle, kwaye isantya se-35.0% sabonwa kwiisampuli zamalahle.Okubaluleke kakhulu, umbane unomcuphi ophantsi kunye namazinga okugqithisa i-56.4% kunye ne-7.7% ngokulandelanayo, kunye nomxholo ophezulu we-0.020 mg / kg.

INGXOXO

Ngokusekwe kwii-PFs ngexesha lokucubungula kunye neentlobo ezimbini zemithombo yokushisa, kwacaca ukuba ukulungiswa kwakuyinyathelo eliphambili elikhokelela ekwandeni kwamanqanaba e-AQ kwimveliso yeti ngamalahle kunye nokusebenza phantsi kwamandla ombane kwaba nefuthe elincinci kumxholo we-AQ. eti.Ngexesha lokusetyenzwa kweti eluhlaza, ukutsha kwamalahle kuvelise umsi omninzi kwinkqubo yokulungisa xa kuthelekiswa nenkqubo yokufudumeza kombane, nto leyo ebonisa ukuba mhlawumbi umsi wawungowona mthombo wongcoliseko lwe-AQ ekudibaneni namahlumelo eti ngoko nangoko ekusetyenzweni kweti, kufana nenkqubo yokuvezwa kwetiyi. iisampulu zebarbecue etshayayo[25].Ukunyuka okuncinci kumxholo we-AQ ngexesha lokuqengqeleka kucebise ukuba i-fumes ebangelwa ukutshiswa kwamalahle ayichaphazeli nje kuphela inqanaba le-AQ ngexesha lesinyathelo sokulungiswa, kodwa nakwindawo yokucubungula ngenxa yokuchithwa kwe-atmospheric.Amalahle nawo asetyenziswa njengomthombo wobushushu ekomisweni kokuqala kunye nokuphinda omiswe, kodwa kula manyathelo mabini umxholo we-AQ unyuke kancinci okanye wehla kancinci.Oku kunokuchazwa yinto yokuba isomisi somoya oshushu esivaliweyo sasigcina iti kude nomsi obangelwa kukutsha kwamalahle[26].Ukuze kubonwe umthombo ongcolisekileyo, amanqanaba e-AQ kwi-atmosfera ahlalutywa, okubangele i-gap ebalulekileyo phakathi kweeworkshop ezimbini.Isizathu esona sizathu salokhu kukuba amalahle asetyenziswe ekulungiseni, okokuqala ukomisa kunye nezigaba zokumisa kwakhona ziza kuvelisa i-AQ ngexesha lokutsha okungaphelelanga.Ezi AQ zaye zabhengezwa kumasuntswana amancinci aqinileyo emva kokutsha kwamalahle kwaye asasazwa emoyeni, ephakamisa amanqanaba ongcoliseko lwe-AQ kwindawo yokusebenzela[15].Ngokuhamba kwexesha, ngenxa yendawo enkulu yendawo ethile kunye nomthamo we-adsorption yeti, la masuntswana emva koko ahlala kumphezulu wamagqabi eti, okukhokelela ekwandeni kwe-AQ kwimveliso.Ke ngoko, ukutshiswa kwamalahle kwakucingelwa ukuba yeyona ndlela ikhokelela kungcoliseko olugqithisileyo lwe-AQ ekusetyenzweni kweti, kunye nomsi ongumthombo wongcoliseko.

Ngokuphathelele ukusetyenzwa kweti ye-oolong, i-AQ yonyuswa phantsi kokulungiswa kwayo yomibini imithombo yobushushu, kodwa umahluko phakathi kwemithombo yobushushu emibini wawubalulekile.Iziphumo ziphinde zacebisa ukuba amalahle njengomthombo wobushushu adlale indima enkulu ekunyuseni izinga le-AQ, kwaye ukulungiswa kwathathwa njengenyathelo eliphambili lokunyusa ungcoliseko lwe-AQ kwi-oolong tea processing esekelwe kwi-PFs.Ngexesha lokulungiswa kweti ye-oolong kunye ne-hybrid yegesi yendalo njengomthombo wobushushu, umgangatho we-AQ wawudodobala ngaphantsi kwe-0.005 mg / kg, eyayifana naleyo yeti eluhlaza ngombane, ebonisa ukuba amandla acocekileyo, njengombane kunye nendalo. igesi, inokunciphisa umngcipheko wokuvelisa ungcoliseko lwe-AQ ekuqhubekeni phambili.

Ngokubhekiselele kwiimvavanyo zesampula, iziphumo zibonise ukuba imeko ye-AQ yongcoliseko yayimbi kakhulu xa kusetyenziswa amalahle njengomthombo wobushushu kunombane, onokuthi ubangelwa ngumphunga wokutsha kwamalahle adibana namagqabi eti kunye nokujikeleza kwindawo yokusebenzela.Nangona kunjalo, nangona kwakucacile ukuba umbane ngowona mthombo wobushushu ococekileyo ngexesha lokulungiswa kweti, kwakusekho ukungcola kwe-AQ kwiimveliso zeti zisebenzisa umbane njengomthombo wobushushu.Imeko ibonakala ifana kancinci nomsebenzi opapashwe ngaphambili apho ukusabela kwe-2-alkenals kunye ne-hydroquinones kunye ne-benzoquinones kwacetyiswa njengendlela enokubakho yeekhemikhali[23], izizathu zoku ziya kuphandwa kuphando lwexesha elizayo.

IZIGQIBO

Kulo msebenzi, imithombo enokwenzeka yokungcola kwe-AQ kwi-tea eluhlaza kunye ne-oolong yaqinisekiswa ngovavanyo oluthelekisayo olusekelwe kwiindlela zokuhlalutya eziphuculweyo ze-GC-MS/MS.Iziphumo zethu zixhasa ngokuthe ngqo ukuba owona mthombo ungcolisekileyo wamanqanaba aphezulu e-AQ yayingumsi obangelwa kukutsha, okungazange kuchaphazele kuphela izigaba zokusetyenzwa kodwa kwachaphazela iindawo zokusebenzela.Ngokungafaniyo nenqanaba lokuqengqeleka kunye nokubuna, apho utshintsho kwinqanaba le-AQ lalingabonakali, izigaba ngokubandakanyeka ngokuthe ngqo kwamalahle kunye neenkuni, ezifana nokulungiswa, yinkqubo ephambili apho ukungcola kwe-AQ kwavuka ngenxa yoqhagamshelwano phakathi kweti. kunye nomsi ngezi zigaba.Ke ngoko, iifutha ezicocekileyo ezifana nerhasi yendalo kunye nombane zacetyiswa njengomthombo wobushushu ekusetyenzweni kweti.Ukongeza, iziphumo zovavanyo zikwabonise ukuba ukungabikho komsi oveliswa kukutsha, kusekho ezinye izinto ezinegalelo ekulandeleni i-AQ ngexesha lokusetyenzwa kweti, ngelixa iimali ezincinci ze-AQ ziye zabonwa kwindibano yocweyo ngamafutha acocekileyo, ekufuneka ephandwe ngakumbi. kuphando lwexesha elizayo.

IMPAHLA NENKQUBO

Ii-reagents, iikhemikhali kunye nemathiriyeli

Umgangatho we-anthraquinone (99.0%) wathengwa kuGqr. Ehrenstorfer GmbH Company (Augsburg, Germany).Umgangatho wangaphakathi we-D8-Anthraquinone (98.6%) wathengwa kwi-C/D/N Isotopes (eQuebec, eCanada).I-Anhydrous sodium sulfate (Na2SO4) kunye ne-magnesium sulfate (MgSO4) (iShanghai, iChina).I-Florisil yanikezelwa yi-Wenzhou Organic Chemical Company (Wenzhou, China).Iphepha le-Mircro-glass fiber (90 mm) lathengwa kwinkampani yakwa-Ahlstrom-munksjö (eHelsinki, eFinland).

Ukulungiselela isampuli

Iisampulu zeti eluhlaza zicutshungulwe ngokulungiswa, ukuqengqeleka, ukomiswa kuqala kunye nokuphinda zomiswe (kusetyenziswa izixhobo ezivaliweyo), ngelixa iisampulu zeti ye-oolong zacutshungulwa ngokubuna, zenza luhlaza (ukugungqa nokuma amagqabi amatsha ngokutshintshanayo), ukulungiswa, ukuqengqeleka, kunye ukomisa.Iisampuli ukusuka kwinqanaba ngalinye ziqokelelwe kathathu kwi-100g emva kokuxuba ngokucokisekileyo.Zonke iisampulu zigcinwe ku-−20 °C ukuze zihlalutywe ngakumbi.

Iisampulu zomoya zaqokelelwa ngephepha le-glass fiber (90 mm) usebenzisa i-samplers volume medium (PTS-100, Qingdao Laoshan Electronic Instrument Company, Qingdao, China) [27], eqhuba kwi-100 L / min kwi-4 h.

Iisampulu eziqinisiweyo zaxutywa nge-AQ kwi-0.005 mg / kg, 0.010 mg/kg, 0.020 mg/kg yamahlumela eti entsha, kwi-0.005 mg/kg, 0.020 mg/kg, 0.050 mg/kg yeti eyomileyo nakwi-0.012 mg/kg (0.5 µg/m3 yesampulu yomoya), 0.036 mg/kg (1.5 µg/m3 yesmaple yomoya), 0.072 mg/kg (3.0 µg/m3 yesampulu yomoya) kwiphepha lokucoca iglasi, ngokulandelelanayo.Emva kokugubha ngokucokisekileyo, zonke iisampuli zishiywe kwi-12 h, zilandelwa ngamanyathelo okukhutshwa kunye nokucoca.

Isiqulatho somswakama sifunyenwe ngokuthatha i-20 g yesampuli emva kokuxuba inyathelo ngalinye, ukufudumeza kwi-105 ° C kwi-1 h, emva koko ukulinganisa kunye nokuphindaphinda kathathu kunye nokuthatha ixabiso eliqhelekileyo kunye nokulwahlula ngobunzima ngaphambi kokufudumeza.

Ukutsalwa kwesampuli kunye nokucoca

Isampula yeti: Ukukhutshwa kunye nokuhlanjululwa kwe-AQ kwiisampuli zeti zenziwa ngokusekelwe kwindlela epapashwe nguWang et al.ngohlengahlengiso oluninzi[21].Ngokufutshane, i-1.5 g yeesampulu zeti yayixutywe kuqala kunye ne-30 μL D8-AQ (2 mg / kg) kwaye ishiywe ukuba imele i-30 min, ize ixutywe kakuhle kunye ne-1.5 mL yamanzi adibeneyo kwaye ishiywe ukuba imele i-30 min.I-15 mL I-20% ye-acetone kwi-n-hexane yongezwa kwiisampuli zeti kunye ne-sonicated ye-15 min.Emva koko iisampuli zixutywe nge-1.0 g MgSO4 kwi-30 s, kwaye i-centrifuged ye-5 min, kwi-11,000 rpm.Emva kokufuduselwa kwi-100 mL yeeflasks ezimile okweperile, i-10 mL yesigaba esiphezulu se-organic yakhukuliseka yaphantse yoma phantsi kwevacuum engama-37 °C.I-5 mL I-2.5% i-acetone kwi-n-hexane iphinde yachithwa isicatshulwa kwiiflasks ezinepear ukuze zihlambuluke.Ikholomu yeglasi (10 cm × 0.8 cm) yayiquka ukusuka ezantsi ukuya phezulu koboya beglasi kunye ne-2g florisil, eyayiphakathi kwamaleko amabini angama-2 cm Na2SO4.Emva koko i-5 mL ye-2.5% ye-acetone kwi-n-hexane ihlanjwe kwangaphambili ikholamu.Emva kokulayisha isisombululo esichithwe kwakhona, i-AQ yahlanjululwa kathathu nge-5 mL, i-10 mL, i-10 mL ye-2.5% ye-acetone kwi-n-hexane.Izinto eziphumayo ezidityanisiweyo zakhutshelwa kwiiflaski ezimile okweperile zaza zajika zatshatyalaliswa zaya kutsho kome ngaphantsi kwe vacuum engama-37 °C.Intsalela eyomisiweyo iye yaphinda yadityaniswa nge-1 mL ye-2.5% ye-acetone kwi-hexane elandelwa kukuhluzwa ngesihluzo sesayizi ye-0.22 µm.Emva koko isisombululo esihlaziyiweyo sixutywe kunye ne-acetonitrile kwi-volume ratio ye-1: 1.Ukulandela inyathelo lokungcangcazela, i-subnatant yasetyenziselwa uhlalutyo lwe-GC-MS/MS.

Isampulu yomoya: Isiqingatha sephepha lefiber, elixutywe nge-18 μL d8-AQ (2 mg / kg), lifakwe kwi-15 mL ye-20% ye-acetone kwi-n-hexane, emva koko i-sonicated 15 min.Isigaba sezinto eziphilayo sahlulwe nge-centrifugation kwi-11,000 rpm kwi-5 min kwaye yonke i-layer ephezulu yasuswa kwi-flask efana ne-pear.Zonke izigaba zendalo ziye zakhutshwa zibe ngumphunga zaphantse zoma phantsi kwevacuum engama-37 °C.I-5 mL ye-2.5% ye-acetone kwi-hexane iphinde yachithwa izicatshulwa zokuhlanjululwa ngendlela efanayo kwiisampuli zeti.

Uhlalutyo lwe-GC-MS/MS

I-Varian 450 yegesi yechromatograph exhotyiswe ngeVarian 300 tandem mass detector (Varian, Walnut Creek, CA, USA) yasetyenziselwa ukwenza uhlalutyo lwe-AQ nge-MS WorkStation version 6.9.3 software.I-Varian Factor Four capillary column VF-5ms (30 m × 0.25 mm × 0.25 μm) yayisetyenziselwa ukwahlukana kwechromatographic.Irhasi ye-carrier, i-helium (> 99.999%), ibekwe kwinqanaba lokuhamba rhoqo kwe-1.0 mL / min kunye negesi yokungqubana kwe-Argon (> 99.999%).Ubushushu be-oven buqale kwi-80 °C kwaye bubambe i-1 min;ukwanda kwi-15 ° C / min ukuya kwi-240 ° C, emva koko yafikelela kwi-260 ° C kwi-20 ° C / min kwaye ibanjwe i-5min.Iqondo lobushushu lomthombo we-ion lalingama-210 °C, kunye nobushushu bomgca wodluliselo wama-280 °C.Umthamo wesitofu wawuyi-1.0 μL.Imiqathango ye-MRM iboniswe kwiThebhile 3.

Agilent 8890 gas chromatograph exhotyiswe Agilent 7000D triple quadrupole mass spectrometer (Agilent, Stevens Creek, CA, USA) yasetyenziswa ukuhlalutya isiphumo ukuhlanjululwa kunye MassHunter version 10.1 software.I-Agilent J & W HP-5ms GC Column (30 m × 0.25 mm × 0.25 μm) yayisetyenziselwa ukwahlukana kwechromatographic.Irhasi yokuthwala, iHelium (> 99.999%), yamiselwa kwinqanaba lokuhamba rhoqo le-2.25 mL/min kunye negesi yokungqubana kweNitrogen (> 99.999%).Ubushushu bomthombo we-ion we-EI buhlengahlengiswe kwi-280 ° C, efanayo nobushushu bomgca wokudlulisa.Ubushushu be-oven buqale ukusuka kwi-80 °C kwaye bubanjwe imizuzu emi-5;iphakanyiswe ngu-15 ° C / min ukuya kwi-240 ° C, emva koko ifike kwi-280 ° C kwi-25 ° C / min kwaye igcinwe kwi-5 min.Imiqathango ye-MRM iboniswe kwiThebhile 3.

Uhlalutyo lwamanani
Umxholo we-AQ kumagqabi amatsha alungiswa kumxholo owomileyo ngokwahlula ngobuninzi bomswakama ukwenzela ukuthelekisa nokuhlalutya amanqanaba e-AQ ngexesha lokucubungula.

Utshintsho lwe-AQ kwiisampulu zeti zavavanywa ngesoftware yeMicrosoft Excel kunye ne-IBM SPSS Statistics 20.

I-processing factor isetyenziswe ukuchaza utshintsho kwi-AQ ngexesha lokucubungula iti.PF = Rl / Rf , apho i-Rf inqanaba le-AQ phambi kwesinyathelo sokucubungula kunye ne-Rl yinqanaba le-AQ emva kwesinyathelo sokucubungula.I-PF ibonisa ukuhla (PF <1) okanye ukunyuka (PF> 1) kwintsalela ye-AQ ngexesha lenyathelo elithile lokucubungula.

I-ME ibonisa ukuhla (ME <1) okanye ukunyuka (ME> 1) ekuphenduleni izixhobo zokuhlalutya, ezisekelwe kumlinganiselo wemithambeka yokulinganisa kwi-matrix kunye ne-solvent ngolu hlobo lulandelayo:

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

Apho i-slopematrix ilithambeka legophe lolungelelwaniso kwi-matrix ehambelana ne-solvent, i-slopesolvent kukuthambeka kwegophe lohlengahlengiso kwisinyibilikisi.

IMIBULELO
Lo msebenzi uxhaswe yiProjekthi enkulu yeSayensi kunye neTekhnoloji kwiPhondo laseZhejiang (2015C12001) kunye neNational Science Foundation yaseChina (42007354).
Ukugqubana kwemidla
Ababhali bavakalisa ukuba abanalo ukungqubana kwemidla.
Amalungelo kunye neemvume
Ilungelo lokushicilela: © 2022 ngu(ababhali).Umntu onikwe iLayisenisi eKhethekileyo uBomi boShicilelo lwezeMfundo, eFayetteville, eGA.Eli nqaku linqaku elivulekileyo lokufikelela lisasazwe phantsi kweLayisensi ye-Creative Commons Attribution (CC BY 4.0), tyelela https://creativecommons.org/licenses/by/4.0/.
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