Abstract
9,10-Anthraquinone (AQ) inosvibisa ine njodzi inogona kuita carcinogenic uye inoitika mutii pasi rese. Iyo yakanyanya kusara muganho (MRL) yeAQ mutei yakatarwa neEuropean Union (EU) ndeye 0.02 mg/kg. Iwo angangove masosi eAQ mukugadzira tii uye nhanho huru dzekuitika kwayo zvakaongororwa zvichibva pane yakagadziridzwa AQ analytical nzira uye gasi chromatography-tandem mass spectrometry (GC-MS/MS) ongororo. Kuenzaniswa nemagetsi senzvimbo yekupisa mugreen tea processing, AQ yakawedzera ne 4.3 kusvika 23.9 nguva mukugadzira tii nemarasha senzvimbo yekupisa, inodarika 0.02 mg/kg, ukuwo AQ level iri munharaunda yakawedzera katatu. Iwo maitiro akafanana akaonekwa mune oolong tii kugadzirisa pasi pekupisa kwemarasha. Matanho ane kusangana kwakananga pakati pemashizha etii uye utsi, sekugadzirisa uye kuomesa, anoonekwa sematanho makuru ekugadzirwa kweAQ mukugadzira tii. Iwo mazinga eAQ akawedzera nekukwira kwekuonana nguva, zvichiratidza kuti yakakwira yeAQ inosvibisa mutii inogona kubva muhutsi hunokonzerwa nemarasha nekupisa. Zvikamu makumi mana kubva kumasangano akasiyana-siyana ane magetsi kana marasha sezvitubu zvekupisa zvakaongororwa, zvakabva ku50.0% -85.0% uye 5.0% -35.0% yekuona uye kudarika mazinga eAQ. Uye zvakare, iyo yakakwira AQ yemukati ye0.064 mg/kg yakaonekwa mune yetii chigadzirwa nemarasha senzvimbo yekupisa, zvichiratidza kuti huwandu hwakanyanya hwekusvibiswa kweAQ muzvigadzirwa zvetii hunogona kupihwa nemarasha.
Keywords: 9,10-Anthraquinone, Tea kugadzira, Marasha, Kusvibiswa sosi
NHUNGAMIDZO
Tii inogadzirwa nemashizha eevergreen shrub Camellia sinensis (L.) O. Kuntze, chimwe chezvinwiwa zvinofarirwa pasi rose nekuda kwekuzorodza kwacho uye hutano hwakanaka. Muna 2020 pasi rose, kugadzirwa kwetii kwakawedzera kusvika pa5,972 miriyoni metric tons, izvo zvakapetwa kaviri mumakore makumi maviri apfuura[1]. Zvichienderana nenzira dzakasiyana dzekugadzirisa, kune marudzi matanhatu makuru etii, kusanganisira yegirinhi, tii nhema, tii yakasviba, oolong tii, tii chena uye yero [2,3]. Kuve nechokwadi chemhando uye kuchengetedzeka kwezvigadzirwa, zvakakosha kwazvo kutarisa mazinga ezvinosvibisa uye kutsanangura kwakabva.

Kuziva kunobva zvinosvibisa, zvakaita sezvisaririra zvemishonga yezvipembenene, simbi dzinorema uye zvimwe zvinosvibisa zvakaita sepolycyclic aromatic hydrocarbons (PAHs), ndiro danho rekutanga rekudzora kusvibiswa. Kumwaya kwakananga kwemakemikari ekugadzira muminda yetii, pamwe nekukukurwa nemhepo kunokonzerwa nemashandiro ari pedyo nemapindu etii, ndiko kunobva masaga emishonga yezvipembenene mutii[4]. Simbi dzinorema dzinogona kuungana mutii uye dzinotungamira kune chepfu, iyo inonyanya kutorwa kubva muvhu, fetiraiza nemhepo[5-7]. Kana zviri kumwe kusvibiswa kunoonekwa zvisingatarisirwe mutii, zvaive zvakaoma kuziva nekuda kwemaitiro akaomarara ekugadzira tii cheni kusanganisira kudyara, kugadzira, kurongedza, kuchengetedza uye kutakura. Iyo PAHs mutii yakabva pakuiswa kwemagetsi emagetsi uye kupiswa kwemafuta anoshandiswa panguva yekugadzira mashizha etii, sehuni nemarasha[8-10].

Munguva yekupisa kwemarasha nehuni, zvinosvibisa zvakaita secarbon oxides zvinogadzirwa[11]. Nekuda kweizvozvo, zvinokwanisika kuti zvisaririra zvezvinosvibisa izvi zvakataurwa pamusoro zviitike muzvigadzirwa zvakagadziriswa, sezviyo, kusvuta nyama nehove dzekatsi, pakupisa kwakanyanya, zvichiunza njodzi kuhutano hwevanhu [12,13]. I-PAHs inokonzerwa nekupisa inotorwa kubva mukupisa kwePAHs iri mumafuta acho pachayo, kuora kwepamusoro-kupisa kwemishonga inonhuhwirira uye maitiro emukomboni pakati pemahara radicals [14]. Kupisa tembiricha, nguva, uye okisijeni yemukati zvinhu zvakakosha zvinokanganisa kutendeuka kwePAHs. Nekuwedzera kwekushisa, zvinyorwa zvePAH zvakatanga kuwedzera uye zvakaderera, uye kukosha kwepamusoro kwakaitika pa800 ° C; Zvinyorwa zvePAH zvakadzikira zvakanyanya kutevera nekuwedzera nguva yekupisa apo yaive pasi pemuganhu unonzi 'nguva yemuganhu', nekuwedzera kweokisijeni mumhepo inopisa, kubuda kwePAHs kwakaderedzwa zvakanyanya, asi oxidation isina kukwana yaizoburitsa maOPAH nezvimwe zvinobva [15]. −17].

9,10-Anthraquinone (AQ, CAS: 84-65-1, Fig. 1), mhepo ine okisijeni inobva kuPAHs [18], inoumbwa nematatu akakomberedzwa. Yakanga yakanyorwa seinobvira carcinogen (Boka 2B) neInternational Agency for Research on Cancer muna 2014[19]. AQ inogona kuchetura kune topoisomerase II cleavage yakaoma uye inhibit hydrolysis yeadenosine triphosphate (ATP) neDNA topoisomerase II, zvichikonzera DNA mbiri-strand breaks, zvinoreva kuti kuratidzwa kwenguva refu pasi peAQ-ine nharaunda uye kusangana kwakananga nehupamhi hweAQ. zvinogona kutungamirira kukukuvadzwa kweDNA, kuchinja uye kuwedzera njodzi yegomarara[20]. Semhedzisiro yakaipa pahutano hwevanhu, iyo AQ yakanyanya kusara muganho (MRL) ye0.02 mg/kg yakaiswa mutii neEuropean Union. Zvinoenderana nezvidzidzo zvedu zvakapfuura, madhipoziti eAQ akakurudzirwa sesosi huru panguva yekurima tii[21]. Zvakare, zvichibva pamhedzisiro yekuedza muIndonesia yakasvibira uye dema tii kugadzirisa, zviri pachena kuti iyo AQ level yakachinja zvakanyanya uye utsi kubva mukugadzira michina yakataurwa sechimwe chezvikonzero zvikuru[22]. Nekudaro, iyo chaiyo mabviro eAQ mukugadzira tii yakaramba isinganzwisisike, kunyangwe mamwe mafungidziro eAQ kemikari nzira akakurudzirwa [23,24], zvichiratidza kuti zvakakosha zvakanyanya kuona zvakakosha zvinokanganisa chikamu cheAQ mukugadzira tii.

Mufananidzo 1. Mushonga wemakemikari weAQ.

Tichifunga nezve tsvagiridzo yekuumbwa kweAQ panguva yekupisa kwemarasha uye njodzi inogona kuitika yemafuta mukugadzira tii, kuyedza kwekuenzanisa kwakaitwa kutsanangura mabatiro ekugadzirisa kupisa masosi paAQ mutii nemhepo, kuongororwa kwehuwandu pane shanduko yezvinyorwa zveAQ. pamatanho akasiyana ekugadzirisa, ayo anobatsira kusimbisa kwakaringana kwakabva, chiitiko chiitiko uye dhigirii reAQ kusvibiswa mukugadzira tii.

RESULTS
Nzira yekusimbisa
Kuenzaniswa nekudzidza kwedu kwekare [21], nzira yekubvisa-mvura-yemvura yakasanganiswa isati yaiswa jekiseni kuGC-MS/MS kuitira kuvandudza kunzwisiswa uye kuchengetedza zvirevo zvezvishandiso. Mumufananidzo 2b, nzira yakagadziridzwa yakaratidza kuvandudzwa kwakakosha mukucheneswa kwemuenzaniso, iyo yakanyungudutsa yakave yakareruka muvara. Mumufananidzo 2a, yakazara scan spectrum (50-350 m / z) yakaratidza kuti mushure mekucheneswa, mutsara wekutanga weMS spectrum wakaderedzwa zviri pachena uye mashoma chromatographic peaks aivepo, zvichiratidza kuti nhamba huru yezvipingamupinyi zvinokanganisa zvakabviswa mushure mekupedzisira. mvura-yemvura kutorwa.

Mufananidzo 2. (a) Full scan spectrum yemuenzaniso musati uye mushure mekucheneswa. (b) Mhedzisiro yekuchenesa yenzira yakagadziridzwa.
Nzira yekusimbisa, kusanganisira mutsara, kupora, muganhu wehuwandu (LOQ) uye matrix effect (ME), inoratidzwa muTebhu 1. Zvinogutsa kuwana mutsara ne coefficient of determination (r2) yakakwirira kudarika 0.998, iyo yakabva ku0.005 kusvika ku 0.2 mg/kg mu tea matrix uye acetonitrile solvent, uye mumhepo sampuli ine huwandu hwe 0.5 kusvika 8 μg/m3.

Kudzoreredzwa kweAQ kwakaongororwa pamatanho matatu akaiswa pakati peyakayerwa uye chaiyo yekumisikidza mune yakaoma tii (0.005, 0.02, 0.05 mg/kg), nhungirwa yetii nyowani (0.005, 0.01, 0.02 mg/kg) uye sampuli yemhepo (0.5, 1.5, 3 μg/m3). Kudzoreredzwa kweAQ mutii kwakatangira pa77.78% kusvika 113.02% mui yakaoma tii uye kubva 96.52% kusvika 125.69% mumapfuti etii, neRSD% yakaderera pane 15%. Kudzoreredzwa kweAQ mumasampuli emhepo kubva pa78.47% kusvika 117.06% neRSD% pazasi 20%. Iyo yakaderera spiked yekumisikidza yakaonekwa seLOQ, yaive 0.005 mg/kg, 0.005 mg/kg uye 0.5 μg/m³ mumapfuti eti, tii yakaoma uye masampuli emhepo, zvichiteerana. Sezvakanyorwa muTable 1, iyo matrix yetii yakaoma uye pfuti yetii yakawedzera zvishoma mhinduro yeAQ, zvichiita kuti ME ye109.0% uye 110.9%. Kana ari matrix emasampuli emhepo, ME yaive 196.1%.

Iwo mazinga eAQ panguva yegirinhi tii kugadzirisa
Nechinangwa chekutsvaga mhedzisiro yezvakasiyana zvekupisa patii uye kugadzirisa nharaunda, batch remashizha matsva rakakamurwa kuita mapoka maviri chaiwo uye rakagadziriswa zvakasiyana mumashopu maviri ekugadzirisa mune rimwe bhizinesi. Rimwe boka rakapiwa magetsi, uye rimwe racho nemarasha.

Sezvinoratidzwa mumufananidzo 3, iyo AQ level ine magetsi semhepo inopisa kubva ku0.008 kusvika 0.013 mg / kg. Munguva yekugadzirisa, kuomeswa kwemashizha etii kunokonzerwa nekugadziriswa mupoto ine tembiricha yakanyanya kwakakonzera kuwedzera kwe9.5% muAQ. Zvadaro, iyo nhanho yeAQ yakaramba iri panguva yekukunguruka kunyangwe kurasikirwa kwejusi, zvichiratidza kuti maitiro emuviri anogona kusakanganisa mwero weAQ mukugadzirisa tii. Mushure mematanho ekutanga ekuomesa, AQ level yakawedzera zvishoma kubva 0.010 kusvika 0.012 mg / kg, ndokuramba ichikwira kusvika 0.013 mg / kg kusvika pakuguma kwekuomeswa zvakare. PFs, iyo yakaratidza zvakanyanya kusiyanisa nhanho imwe neimwe, yaiva 1.10, 1.03, 1.24, 1.08 mukugadzirisa, kukunguruka, kutanga kuomesa uye kuomesa zvakare, maererano. Mhedzisiro yePFs yakaratidza kuti kugadzirisa pasi pesimba remagetsi kwakakanganisa zvishoma pamazinga eAQ mutii.

Mufananidzo 3. Chiyero cheAQ panguva yegreen tea kugadzirisa nemagetsi nemarasha sezvitubu zvekupisa.
Panyaya yemarasha senzvimbo yekupisa, iyo AQ yemukati yakawedzera zvakanyanya panguva yekugadzira tii, ichikwira kubva pa0.008 kusvika 0.038 mg/kg. 338.9% AQ yakawedzerwa mukugadzirisa nzira, inosvika 0.037 mg / kg, iyo yakapfuura kure MRL ye 0.02 mg / kg yakagadzwa neEuropean Union. Munguva yekutenderedza nhanho, nhanho yeAQ ichiri kuwedzera ne5.8% kunyangwe iri kure nemuchina wekugadzirisa. Mukutanga kuomesa uye kuomesa zvakare, iyo AQ yemukati yakawedzera zvishoma kana kuderera zvishoma. MaPF anoshandisa marasha senzvimbo yekupisa mukugadzirisa, kupeta kwekutanga kuomesa uye kuomesa zvakare aive 4.39, 1.05, 0.93, uye 1.05, zvichiteerana.

Kuti uwedzere kuona hukama pakati pekupisa kwemarasha uye kusvibiswa kweAQ, nyaya dzakasimwa (PMs) mumhepo mumasangano pasi pezvinhu zvose zvinopisa zvakaunganidzwa kuti zviongororwe nemhepo, sezvakaratidzwa mumufananidzo 4. Nhamba yeAQ yePM ine marasha se iyo inopisa sosi yaive 2.98 μg/m3, iyo yaive yakapetwa katatu kupfuura iyo ine magetsi 0.91 μg/m3.

Mufananidzo 4. Mazinga eAQ munharaunda ine magetsi nemarasha semhepo inopisa. * Inoratidza mutsauko wakakura mumazinga eAQ mumasampuli (p <0.05).

Iwo mazinga eAQ panguva ye oolong tii kugadzirisa Oolong tii, inonyanya kugadzirwa muFujian neTaiwan, imhando yetii yakaviriswa zvishoma. Kuti uwedzere kuona nhanho huru dzekuwedzera AQ nhanho uye mhedzisiro yemafuta akasiyana, iro batch rakafanana remashizha matsva rakagadzirwa kuita oolong tii ine marasha uye echisikigo gasi-yemagetsi hybrid sezvitubu zvekupisa, panguva imwe chete. Iwo maAQ mazinga muoolong tea processing uchishandisa zvakasiyana-siyana zvinopisa zvinoratidzwa muFig. 5. Kune oolong tea processing ine natural gas-electric hybrid, maitiro eAQ level akanga achidzika pasi pe0.005 mg/kg, iyo yakanga yakafanana neyo mu green tea. nemagetsi.

Mufananidzo 5. Chiyero cheAQ panguva ye oolong tii yekugadzirisa negasi-yemagetsi musanganiswa uye marasha semhepo inopisa.

Nemarasha senzvimbo yekupisa, mazinga eAQ mumatanho maviri ekutanga, kusvava uye kugadzira girinhi, aive akafanana neakasikwa gasi-magetsi musanganiswa. Nekudaro, maitiro aitevera kusvika kugadziriswa kwakaratidza gap rakawedzera zvishoma nezvishoma, panguva iyo iyo AQ level yakakwira kubva pa0.004 kusvika 0.023 mg/kg. Iyo nhanho mune yakarongedzwa nhanho yekutenderera yakadzikira kusvika 0.018 mg/kg, izvo zvinogona kunge zviri nekuda kwekurasikirwa kwetii muto unotakura zvimwe zveAQ zvinosvibisa. Mushure mechikamu chekukunguruka, chiyero muchikamu chekuomesa chakawedzera kusvika 0.027 mg / kg. Mukusvava, kugadzira girini, kugadzirisa, kurongedzerwa nekuomesa, maPF aive 2.81, 1.32, 5.66, 0.78, uye 1.50, zvichiteerana.

Kuitika kweAQ mune zvigadzirwa zvetii zvine akasiyana kupisa masosi

Kuti uone migumisiro yeAQ yetiyi ine zvakasiyana-siyana zvekupisa, 40 tea samples kubva ku tea workshops vachishandisa magetsi kana marasha sezvitubu zvekupisa zvakaongororwa, sezvinoratidzwa muTable 2. Kuenzaniswa nekushandisa magetsi sechitubu chekupisa, marasha aiva nemafuta akawanda. Detective rates (85.0%) nehupamhi hweAQ level ye0.064 mg/kg, zvichiratidza kuti zvaive nyore kukonzera AQ kusvibiswa nehutsi hunogadzirwa ne kupiswa kwemarasha, uye chiyero che35.0% chakaonekwa mumasampuli emarasha. Kunyanya kuoneka, magetsi aive neakaderera detective uye kuwedzera kwemazinga e56.4% uye 7.7% maererano, nehuwandu hwehuwandu hwe0.020 mg / kg.

HURUKURO

Zvichienderana nePFs panguva yekugadziriswa nemhando mbiri dzekupisa, zvaive pachena kuti kugadzirisa yaive nhanho huru yakatungamira kuwedzera kwemazinga eAQ mukugadzirwa kwetii nemarasha uye kugadzirisa pasi pesimba remagetsi kwakakanganisa zvishoma pane zvirimo muAQ. mu tea. Munguva yekugadzira green tea, kupiswa kwemarasha kwakaburitsa utsi hwakawanda mukugadzirisa zvichienzaniswa nemagetsi ekudziya, zvichiratidza kuti pamwe utsi ndihwo hwainyanya kukonzera kusvibisa kweAQ kubva pakusangana nenhungirwa yetii ipapo mukugadzira tii, zvakafanana nemaitiro ekufumura. sampuli dzebarbecue dzakaputa[25]. Kuwedzera kudiki kwemukati weAQ panguva yekutenderedza kwakaratidza kuti utsi hunokonzerwa nekupisa kwemarasha hahuna kungokanganisa nhanho yeAQ panguva yedanho rekugadzirisa, asiwo munzvimbo yekugadzirisa nekuda kwekuiswa kwemhepo. Marasha aishandiswawo senzvimbo yekupisa mukutanga kuomeswa uye kuomesa zvakare, asi mumatanho maviri aya zvinyorwa zveAQ zvakawedzera zvishoma kana kuderera zvishoma. Izvi zvinogona kutsanangurwa nenyaya yekuti muomesi wemhepo inopisa waichengeta tii kure neutsi hunokonzerwa nekupisa kwemarasha[26]. Kuti uone kwakabva kusvibisa, mazinga eAQ mumhepo akaongororwa, zvichiita kuti pave nemukaha wakakura pakati pemawekishopu maviri. Chikonzero chikuru cheizvi ndechekuti marasha anoshandiswa mukugadzirisa, kutanga kuomeswa uye kuomeswazve matanho aizogadzira AQ panguva yekupisa kusina kukwana. Aya maAQ akabva adsorbed muzvikamu zvidiki zvezvakaoma mushure mekupisa kwemarasha uye akapararira mumhepo, zvichisimudza mazinga ekusvibiswa kweAQ munzvimbo yemusangano[15]. Nekufamba kwenguva, nekuda kweiyo yakakura nzvimbo yepasi uye adsorption kugona kwetii, aya maturu akabva agara pamusoro pemashizha etii, zvichikonzera kuwedzera kweAQ mukugadzira. Naizvozvo, kupisa kwemarasha kwaifungidzirwa kuti ndiyo nzira huru inotungamira mukusvibiswa kwakanyanyisa kweAQ mukugadziriswa kwetii, nehutsi huri huchikonzera kusvibiswa.

Kana iri oolong tii yekugadzirisa, AQ yakawedzerwa pasi pekugadziriswa nezvose zviri zviviri kupisa masosi, asi mutsauko uripo pakati pezviviri zvekupisa sosi waive wakakosha. Mhedzisiro yacho yakaratidzawo kuti marasha senzvimbo yekupisa yakaita basa rakakura mukuwedzera AQ level, uye kugadzirisa kwacho kwakaonekwa senhanho huru yekuwedzera kusvibiswa kweAQ muoolong tii processing yakavakirwa paPFs. Munguva yeoolong tii yekugadzirisa negasi-yemagetsi hybrid senzvimbo yekupisa, maitiro eAQ level akange achidzika pasi pe0.005 mg/kg, iyo yakafanana neiyo mugirini tii nemagetsi, zvichiratidza kuti simba rakachena, semagetsi uye zvakasikwa. gasi, inogona kuderedza njodzi yekugadzira AQ zvinosvibisa kubva pakugadziriswa.

Kana iri sampling bvunzo, mhedzisiro yakaratidza kuti mamiriro ekusvibiswa kweAQ akanyanya kuipa kana ukashandisa marasha sechitubu chekupisa kwete magetsi, izvo zvinogona kunge zvichikonzerwa nekupisa kwemarasha kunosangana nemashizha etii uye kutenderera kubasa. Nekudaro, kunyangwe zvaive pachena kuti magetsi ndiwo akanyanya kupisa sosi panguva yekugadzira tii, pakanga pachine AQ inosvibisa muzvigadzirwa zvetii vachishandisa magetsi senzvimbo yekupisa. Mamiriro acho anoita seakada kufanana nebasa rakamboburitswa umo maitiro e2-alkenals ane hydroquinones uye benzoquinones akakurudzirwa seanogona kuita kemikari nzira[23], zvikonzero zveizvi zvichaongororwa mune ramangwana tsvagiridzo.

MHEDZISO

Mubasa iri, zvingangobva kusvibiswa kweAQ mugirini uye oolong tii zvakasimbiswa nekuenzanisa kuyedza kwakavakirwa pakuvandudzwa kweGC-MS/MS nzira dzekuongorora. Zvatakawana zvakatsigira zvakananga kuti iyo huru yekusvibisa kwemazinga akakwira eAQ yaive utsi wakakonzerwa nekupisa, izvo zvisina kungokanganisa matanho ekugadzirisa chete asiwo zvakakanganisa nharaunda dzemusangano. Kusiyana mumatanho ekukunguruka uye kuoma, uko shanduko muchikamu cheAQ yakanga isingaonekwe, matanho ane kubatanidzwa kwakananga kwemarasha nehuni, sekugadzirisa, ndiyo nzira huru iyo AQ kusvibiswa kwakasimuka nekuda kwehuwandu hwekubatana pakati petii. uye utsi panguva idzi. Naizvozvo, mafuta akachena akadai segasi rechisikigo nemagetsi akakurudzirwa senzvimbo yekupisa mukugadzira tii. Pamusoro pezvo, mhedzisiro yekuyedza yakaratidzawo kuti mukushaikwa kwehutsi hunogadzirwa nekupisa, pakanga pachine zvimwe zvinhu zvaibatsira kutsvaga AQ panguva yekugadzira tii, nepo zvidiki zveAQ zvakaonekwa mumusangano nemafuta akachena, izvo zvinofanirwa kuongororwa zvakare. mukutsvakurudza mune ramangwana.

ZVINHU UYE NZIRA

Reagents, makemikari uye zvinhu

Anthraquinone standard (99.0%) yakatengwa kubva kuna Dr. Ehrenstorfer GmbH Company (Augsburg, Germany). D8-Anthraquinone yemukati mwero (98.6%) yakatengwa kubva kuC/D/N Isotopes (Quebec, Canada). Anhydrous sodium sulfate (Na2SO4) uye magnesium sulfate (MgSO4) (Shanghai, China). Florisil yakapihwa neWenzhou Organic Chemical Company (Wenzhou, China). Mircro-glass fiber paper (90 mm) yakatengwa kubva kukambani yeAhlstrom-munksjö (Helsinki, Finland).

Kugadzirira kwemuenzaniso

Iwo green tea samples dzakagadziriswa nekugadzirisa, kukunguruka, kutanga kuomesa uye kuomesa zvakare (uchishandisa midziyo yakavharirwa), nepo oolong tii samples dzakagadziriswa nekuoma, kuita girinhi (kuzununguka uye kumira mashizha matsva neimwe nzira), kugadzirisa, kurongedza, uye. kuomesa. Mienzaniso kubva pane imwe neimwe nhanho yakaunganidzwa katatu pa 100g mushure mekunyatsosanganiswa. Masampuli ese akachengetwa pa −20 °C kuti awedzere kuongororwa.

Masampuli emhepo akaunganidzwa negirazi fiber paper (90 mm) achishandisa medium volume samplers (PTS-100, Qingdao Laoshan Electronic Instrument Company, Qingdao, China) [27], ichimhanya pa100 L / min ye4 h.

Samples dzakasimbiswa dzakaiswa spiked neAQ pa0.005 mg/kg, 0.010 mg/kg, 0.020 mg/kg yezvipfukuto zvinyoro, pa0.005 mg/kg, 0.020 mg/kg, 0.050 mg/kg yetii yakaoma uye pa0.012 mg/kg (0.5 µg/m3 yemuenzaniso wemhepo), 0.036 mg/kg (1.5 µg/m3 yemhepo smaple), 0.072 mg/kg (3.0 µg/m3 yesample yemhepo) yegirazi sefa bepa, zvichiteerana. Mushure mokuzunungusa zvakakwana, sampuli dzose dzakasiiwa kwe12 h, dzichiteverwa nekutora uye matanho ekuchenesa.

Hunyoro hwehunyoro hwakawanikwa nekutora 20 g yemuenzaniso mushure mekusanganisa nhanho imwe neimwe, kupisa pa105 ° C kwe1 h, ipapo kuyera nekudzokorora katatu uye kutora kukosha kweavhareji nekuipatsanura nehuremu isati yapisa.

Sample kutorwa uye kuchenesa-up

Sample yetii: Kudhirowa uye kucheneswa kweAQ kubva kune tii samples kwakaitwa zvichibva pane yakadhindwa nzira kubva kuna Wang et al. nemaitiro akati wandei[21]. Nenguva pfupi, 1.5 g yetii samples yakatanga kusanganiswa ne 30 μL D8-AQ (2 mg / kg) uye yakasara kuti imire kwemaminitsi makumi matatu, uye yakanyatsosanganiswa ne 1.5 mL yemvura yakasvibiswa uye yakasara kuti imire kwemaminitsi makumi matatu. 15 mL 20% acetone mu n-hexane yakawedzerwa kumasampuli etii uye sonicated kwemaminitsi gumi nemashanu. Zvadaro sampuli dzakasvibiswa ne 1.0 g MgSO4 ye 30 s, uye centrifuged ye 5 min, pa 11,000 rpm. Mushure mekuendeswa kune 100 mL maflasks akaita sepear, 10 mL yekumusoro organic phase yakapfachukira kusvika pakuoma pasi pekutsvaira pa37 ° C. 5 mL 2.5% acetone mu n-hexane yakanyungudusa zvakare iyo yakatorwa mumaflask akaita sepear kuti icheneswe. Girazi mbiru (10 cm × 0.8 cm) yaisanganisira kubva pasi kusvika kumusoro kwegirazi mvere uye 2g florisil, iyo yaiva pakati pezvikamu zviviri zve 2 cm Na2SO4. Zvino 5 mL ye2.5% acetone mu n-hexane yakafanogeza mbiru. Mushure mekurodha mhinduro yakanyungudika, AQ yakaburitswa katatu ne5 mL, 10 mL, 10 mL ye2.5% acetone mun-hexane. Maeluate akasanganiswa akaendeswa kune maflasks akaita sepear uye akaputika kusvika pakuoma pasi pevacuum pa37 ° C. Iyo yakaomeswa yakasara yakazogadziriswa ne1 mL ye2.5% acetone muhexane ichiteverwa nekusefa kuburikidza ne0.22 µm pore saizi sefa. Zvadaro mhinduro yakagadziriswa yakasanganiswa neacetonitrile pahuwandu hwehuwandu hwe1: 1. Kutevera danho rekuzungunutsa, iyo subnatant yakashandiswa kuongororwa kweGC-MS/MS.

Muenzaniso wemhepo: Hafu yepepa refiber, yakadonha ne 18 μL d8-AQ (2 mg / kg), yakanyudzwa mu 15 mL ye20% acetone mu n-hexane, uye yakanyungudutswa kwemaminitsi gumi nemashanu. Iyo organic phase yakaparadzaniswa ne centrifugation pa 11,000 rpm ye 5 min uye iyo yese yekumusoro layer yakabviswa mufurasiki yakaita pear. Ese organic nhanho akafemeswa kusvika pakuoma pasi pevacuum pa37 °C. 5 mL ye2.5% acetone muhexane yakanyungudusa zvakare zvinyorwa zvekunatsa nenzira imwechete seyemumasamples etii.

GC-MS/MS kuongorora

Varian 450 gasi chromatograph ine Varian 300 tandem mass detector (Varian, Walnut Creek, CA, USA) yakashandiswa kuita ongororo yeAQ neMS WorkStation version 6.9.3 software. Varian Factor Four capillary column VF-5ms (30 m × 0.25 mm × 0.25 μm) yakashandiswa kuparadzanisa chromatographic. Iyo gasi inotakura, helium (> 99.999%), yakaiswa pachiyero chekuyerera che 1.0 mL/min nekudhumhana gasi reArgon (> 99.999%). Kupisa kwevheni kwakatanga kubva ku80 °C uye kwakabata 1 min; yakawedzera pa15 ° C / min kusvika 240 ° C, ndokuzosvika 260 ° C pa20 ° C / min uye yakabata 5min. Tembiricha yeiyo ion sosi yaive 210 ° C, pamwe netembiricha yekutamisa ye280 ° C. Huwandu hwejekiseni hwaive 1.0 μL. Mamiriro eMRM anoratidzwa muTafura 3.

Agilent 8890 gasi chromatograph yakashongedzerwa neAgilent 7000D katatu quadrupole mass spectrometer (Agilent, Stevens Creek, CA, USA) yakashandiswa kuongorora maitiro ekuchenesa neMassHunter shanduro 10.1 software. Agilent J&W HP-5ms GC Column (30 m × 0.25 mm × 0.25 μm) yakashandiswa kuparadzanisa chromatographic. Iyo gasi inotakura, Helium (> 99.999%), yakaiswa pachiyero chekuyerera che2.25 mL/min nekudhumhana gasi reNitrogen (> 99.999%). Iyo tembiricha yeEI ion sosi yakagadziridzwa pa280 ° C, yakafanana neyekutamisa mutsara tembiricha. Kupisa kwevheni kwakatanga kubva ku80 °C uye kwakabatwa kwemaminitsi mashanu; yakasimudzwa ne15 °C/min kusvika 240 °C, ndokuzosvika 280 °C pa25 °C/min uye yakachengetedzwa kwemaminitsi mashanu. Mamiriro eMRM anoratidzwa muTafura 3.

Statistical analysis
Iyo AQ yemukati mumashizha matsva yakagadziriswa kuti iome zvinhu zviri mukati nekukamurwa nehunyoro hwemukati kuitira kuenzanisa uye kuongorora mazinga eAQ panguva yekugadziriswa.

Shanduko dzeAQ mumasampuli etii dzakaongororwa neMicrosoft Excel software uye IBM SPSS Statistics 20.

Processing factor yakashandiswa kutsanangura shanduko muAQ panguva yekugadzira tii. PF = Rl/Rf , uko Rf ndiyo nhanho yeAQ isati yatanga danho uye Rl ndiyo nhanho yeAQ mushure medanho rekugadzirisa. PF inoratidza kudzikira (PF <1) kana kuwedzera (PF> 1) muAQ yakasara panguva yedanho rekugadzirisa.

ME inoratidza kuderera (ME <1) kana kuwedzera (ME> 1) mukupindura kune zvinyorwa zvekuongorora, izvo zvinoenderana nereshiyo yemateru ekugadzirisa mumatrix uye solvent sezvinotevera:

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

Apo slopematrix iri mutsetse we calibration curve mune matrix-inofananidzwa solvent, slopesolvent ndiyo mutsetse we calibration curve mu solvent.

MUTONGO
Iri basa rakatsigirwa neScience uye Technology Major Project muZhejiang Province (2015C12001) uye National Science Foundation yeChina (42007354).
Kupokana kwechido
Vanyori vanotaura kuti havana kupesana kwechido.
Kodzero nemvumo
Copyright: © 2022 nemunyori(va) Exclusive Licensee Maximum Academic Press, Fayetteville, GA. Ichi chinyorwa chinyorwa chekupinda pachena chakagoverwa pasi peCreative Commons Attribution License (CC BY 4.0), shanyira https://creativecommons.org/licenses/by/4.0/.
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