Abstract
9,10-Anthraquinone (AQ) waa wasakh leh khatar ka iman karta kansarka waxayna ku dhacdaa shaaha adduunka oo dhan. Xadka ugu badan ee hadhaaga (MRL) ee AQ ee shaaha ay dejiyeen Midowga Yurub (EU) waa 0.02 mg/kg. Ilaha suurtogalka ah ee AQ ee diyaarinta shaaha iyo marxaladaha ugu muhiimsan ee ay dhacdo ayaa la baadhay iyada oo lagu salaynayo habka falanqaynta AQ ee la beddelay iyo falanqaynta gaaska chromatography-tandem mass spectrometry (GC-MS/MS). Marka la barbar dhigo koronta sida isha kulaylka ee farsamaynta shaaha cagaaran, AQ wuxuu kordhay 4.3 ilaa 23.9 jeer shaaha warshadaynta dhuxusha sida isha kulaylka, oo aad uga badan 0.02 mg/kg, halka heerka AQ ee deegaanka uu saddex jibaarmay. Isbeddel la mid ah ayaa lagu arkay warshadaynta shaaha oolong ee kulaylka dhuxusha. Tallaabooyinka xiriirka tooska ah ee u dhexeeya caleemaha shaaha iyo qiiqa, sida hagaajinta iyo qalajinta, ayaa loo tixgeliyaa inay yihiin tallaabooyinka ugu muhiimsan ee wax soo saarka AQ ee diyaarinta shaaha. Heerarka AQ waxay kordheen kor u kaca wakhtiga xidhiidhka, taas oo soo jeedinaysa in heerarka sare ee wasakhowga AQ ee shaaha laga yaabo inay ka soo baxaan qiiqa ay sababaan dhuxusha iyo gubashada. Afartan muunado oo laga soo qaatay aqoon-is-weydaarsiyo kala duwan oo leh koronto ama dhuxul sida ilaha kulaylka ayaa la falanqeeyay, waxay u dhexeysay 50.0% -85.0% iyo 5.0% -35.0% si loo ogaado oo ay dhaafto heerka AQ. Intaa waxaa dheer, ugu badnaan AQ content ee 0.064 mg / kg ayaa lagu arkay sheyga shaaha leh dhuxusha sida isha kulaylka, taas oo muujinaysa in heerka sare ee wasakhowga AQ ee alaabta shaaha ay u badan tahay in ay ka qayb qaataan dhuxusha.
Erayada furaha: 9,10-Anthraquinone, Shaaha farsamaynta, Dhuxusha, isha faddaraynta
HORDHAC
Shaaha laga soo saaro caleemaha geedka weligood cagaarka ah ee Camellia sinensis (L.) O. Kuntze, waa mid ka mid ah cabitaannada caanka ah ee adduunka oo dhan sababtoo ah dhadhanka macaan iyo faa'iidooyinka caafimaad. 2020 caalamka, wax soo saarka shaaha ayaa kordhay ilaa 5,972 milyan metrik ton, taasoo labanlaabantay 20kii sano ee la soo dhaafay[1]. Iyada oo ku saleysan habab kala duwan oo loo farsameeyo, waxaa jira lix nooc oo shaaha ah, oo ay ku jiraan shaaha cagaaran, shaaha madow, shaaha madow, shaaha oolong, shaaha cad iyo shaaha jaalaha ah[2,3]. Si loo hubiyo tayada iyo badbaadada alaabta, aad bay muhiim u tahay in la kormeero heerarka wasakhowga iyo qeexida asalka.

Aqoonsiga ilaha wasakhaysan, sida haraaga sunta cayayaanka, biraha culus iyo wasakhowga kale sida polycyclic aromatic hydrocarbons (PAHs), waa talaabada koowaad ee lagu xakameynayo wasakhda. Ku buufinta tooska ah ee kiimikooyinka synthetic ee beeraha shaaha, iyo sidoo kale qulqulka hawada ee ka dhasha hawlgallada u dhow jardiinooyinka shaaha, ayaa ah isha ugu weyn ee haraaga sunta cayayaanka ee shaaha[4]. Biraha culusi waxay ku urursan karaan shaaha waxayna u horseedi karaan sun, kuwaas oo inta badan laga helo ciidda, bacriminta iyo jawiga[5-7]. Marka laga hadlayo wasakhowga kale ee si lama filaan ah ugu soo baxay shaaha, aad ayay u adkeyd in la garto iyadoo ay ugu wacan tahay hababka adag ee silsiladda shaaha wax soo saarka oo ay ka mid yihiin beerista, habaynta, baakadaha, kaydinta iyo gaadiidka. PAH-yada shaaha ku jira waxa ay ka yimaaddeen qiiqa baabuurta oo la dhigo iyo gubista shidaalka la isticmaalo inta lagu jiro habaynta caleenta shaaha, sida xaabada iyo dhuxusha[8-10].

Inta lagu jiro gubashada dhuxusha iyo xaabada, wasakhaha sida kaarboon oxides ayaa la sameeyaa[11]. Natiijo ahaan, waxay u nugushahay hadhaaga wasakhahaas aan kor ku soo sheegnay inay ku dhacaan alaabta la warshadeeyay, sida badarka, hilibka la dhuuqo iyo kalluunka bisadaha, heerkul sare, taasoo khatar ku ah caafimaadka bini'aadamka[12,13]. PAH-yada uu keeno gubashada waxay ka soo jeedaan isbeddelka PAHs ee ku jira shidaalka laftiisa, heerkulka sare ee isku-dhafka udgoonka iyo falcelinta isku-dhafka ah ee u dhexeeya xagjirrada xorta ah[14]. Heerkulka gubashada, wakhtiga, iyo waxa ku jira ogsijiinta waa arrimo muhiim ah oo saameeya beddelka PAHs. Korodhka heerkulku, waxa ku jira PAHs marka hore way korodhay ka dibna hoos u dhacay, qiimaha ugu sarreeyaa wuxuu dhacay 800 °C; Waxyaalaha PAHs ayaa si aad ah hoos ugu dhacay si loo raad raaco iyada oo korodhay wakhtiga gubashada markii ay ka hoosaysay xadka loo yaqaan 'waqtiga xadka', iyada oo korodhka oksijiinta ku jirta hawada gubanaysa, sii daynta PAHs ayaa si aad ah hoos ugu dhacday, laakiin oksaydheynta aan dhamaystirnayn waxay soo saari doontaa OPAHs iyo waxyaalo kale. -17].

9,10-Anthraquinone (AQ, CAS: 84-65-1, Jaantuska 1), oksijiin ka kooban PAHs [18], waxay ka kooban tahay saddex wareeg oo isku dhafan. Waxaa lagu liis gareeyay sida kansarka suurtogalka ah (Kooxda 2B) ee Hay'adda Caalamiga ah ee Cilmi-baarista Kansarka 2014[19]. AQ waxay ku sumayn kartaa topoisomerase II cleavage complex oo waxay joojin kartaa hydrolysis of adenosine triphosphate (ATP) by DNA topoisomerase II, taasoo keenta DNA laba-xarig jajab ah, taas oo macnaheedu yahay in soo-gaadhista muddada-dheer ee hoos yimaada deegaanka AQ-ku jira iyo xiriir toos ah oo lala yeesho heerka sare ee AQ waxay u horseedi kartaa burbur DNA, beddelaad iyo kordhinta halista kansarka[20]. Sida saamaynta taban ee caafimaadka bini'aadamka, xadka ugu sarreeya ee AQ (MRL) ee 0.02 mg/kg ayaa shaaha u dejiyay Midowga Yurub. Marka loo eego daraasadadeenii hore, kaydka AQ ayaa loo soo jeediyay inay yihiin isha ugu weyn inta lagu jiro beeritaanka shaaha[21]. Sidoo kale, iyadoo lagu saleynayo natiijooyinka tijaabada ah ee ka shaqeynta cagaarka iyo shaaha madow ee Indonesian, waxaa muuqata in heerka AQ uu si weyn u bedelay qiiqa ka soo baxa qalabka farsamaynta ayaa lagu soo jeediyay mid ka mid ah sababaha ugu waaweyn[22]. Si kastaba ha ahaatee, asalka saxda ah ee AQ ee diyaarinta shaaha ayaa weli ah mid la fahmi karo, inkastoo qaar ka mid ah mala-awaalka dariiqa kiimikada AQ la soo jeediyay [23,24], taasoo muujineysa inay aad muhiim u tahay in la go'aamiyo arrimaha muhiimka ah ee saameeya heerka AQ ee habka shaaha.

Jaantuska 1. Qaabka kiimikada ee AQ.

Marka la eego cilmi-baarista ku saabsan samaynta AQ inta lagu jiro gubashada dhuxusha iyo khatarta suurtagalka ah ee shidaalka ee farsamaynta shaaha, tijaabo isbarbardhig ah ayaa la sameeyay si loo sharaxo saameynta ka-hortagga ilaha kulaylka ee AQ ee shaaha iyo hawada, falanqaynta qiyaasta ee isbeddelada AQ Tallaabooyin habaysan oo kala duwan, kuwaas oo waxtar u leh xaqiijinta asalka saxda ah, qaabka dhacdada iyo heerka wasakhowga AQ ee habaynta shaaha.

NATIIJADA
Xaqiijinta habka
Marka la barbardhigo daraasaddeennii hore [21], nidaamka soo saarista dareeraha-dareere ah ayaa la isku daray ka hor inta aan la durin GC-MS/MS si loo hagaajiyo dareenka loona ilaaliyo weedhaha qalabka. Jaantuska 2b, habka la wanaajiyay ayaa muujiyay horumar la taaban karo oo lagu nadiifinayo muunada, dareeruhu wuxuu noqday midab khafiif ah. Jaantuska 2a, sawir buuxa oo sawir ah (50-350 m/z) ayaa muujiyay in nadiifinta ka dib, xariiqda asaasiga ah ee MS spectrum ay hoos u dhacday si cad oo yar yar oo koromografi ah ayaa la heli karaa, taas oo muujinaysa in tiro badan oo ka mid ah xeryahooda faragelinta laga saaray ka dib soo saarista dareeraha ah.

Jaantuska 2. (a) Sawirka buuxa ee muunada ka hor iyo ka dib nadiifinta. (b) Saamaynta nadiifinta ee habka la hagaajiyay.
Xaqiijinta habka, oo ay ku jiraan toosnaanta, soo kabashada, xaddidaadda tirada (LOQ) iyo saameynta matrixka (ME), ayaa lagu muujiyay shaxda 1. Waa wax lagu qanco in la helo linearity ee isku-dhafka go'aaminta (r2) ee ka sarreeya 0.998, kaas oo u dhexeeya 0.005 ilaa 0.2 mg/kg ee shaaha shaaha iyo dareeraha acetonitrile, iyo muunada hawada oo leh 0.5 ilaa 8 μg/m3.

Dib u soo kabashada AQ waxaa lagu qiimeeyay saddex xajmiyeed oo udhaxeeya qiyaasta iyo qiyaasta dhabta ah ee shaaha qalalan (0.005, 0.02, 0.05 mg/kg), caleemaha shaaha cusub (0.005, 0.01, 0.02 mg/kg) iyo muunada hawada (0.5, 1.5, 3). μg/m3). Soo kabashada AQ ee shaaha waxay u dhaxaysay 77.78% ilaa 113.02% shaaha qalalan iyo 96.52% ilaa 125.69% caleemaha shaaha, iyadoo RSD% ay ka hooseyso 15%. Soo kabashada AQ ee muunada hawada waxay u dhaxaysay 78.47% ilaa 117.06% iyadoo RSD% ka hooseyso 20%. Xoojinta ugu hoosaysa ayaa loo aqoonsaday sida LOQ, kuwaas oo ahaa 0.005 mg/kg, 0.005 mg/kg iyo 0.5 μg/m³ ee caleemaha shaaha, shaaha qalalan iyo muunadaha hawada, siday u kala horreeyaan. Sida ku qoran shaxda 1, jaantuska shaaha qalalan iyo caleemaha shaaha wax yar ayaa kordhiyey jawaabta AQ, taasoo keentay ME ee 109.0% iyo 110.9%. Marka loo eego shaxanka muunadaha hawada, ME wuxuu ahaa 196.1%.

Heerarka AQ inta lagu jiro farsamaynta shaaha cagaaran
Iyada oo ujeedadu tahay in la ogaado saamaynta ilaha kulaylka ee kala duwan ee shaaha iyo deegaanka warshadaynta, dufcad caleemaha cusub ayaa loo qaybiyay laba kooxood oo gaar ah waxaana si gaar ah looga baaraandegay laba aqoon-is-weydaarsiyo habayn oo isku mid ah. Koox waxa la siinayay koronto, kooxda kalena dhuxul.

Sida ku cad sawirka 3, heerka AQ ee korantada sida isha kulaylka ayaa u dhaxaysay 0.008 ilaa 0.013 mg/kg. Inta lagu jiro habka hagaajinta, dubandhicirka caleemaha shaaha ee ay sababtay farsamaynta dheriga heerkulka sare leh waxay keentay 9.5% korodhka AQ. Kadibna, heerka AQ ayaa ku haray inta lagu guda jiro geeddi-socodka duubista inkastoo lumitaanka casiirka, soo jeedinta in hababka jireed aysan saameyn ku yeelan karin heerka AQ ee habka shaaha. Tallaabooyinka qalajinta ee ugu horreeya ka dib, heerka AQ wuxuu wax yar ka kordhay 0.010 ilaa 0.012 mg / kg, ka dibna wuxuu sii waday inuu kordho 0.013 mg / kg ilaa dhammaadka dib-u-qallajinta. PF-yada, kuwaas oo si weyn u muujiyay kala duwanaanshaha tallaabo kasta, waxay ahaayeen 1.10, 1.03, 1.24, 1.08 hagaajinta, duubista, qalajinta ugu horeysa iyo dib u qalajinta, siday u kala horreeyaan. Natiijooyinka PF-yadu waxay soo jeediyeen in ka shaqaynta tamarta korantada ay saameyn yar ku yeelato heerarka AQ ee shaaha.

Jaantuska 3. Heerka AQ inta lagu jiro farsamaynta shaaha cagaaran ee koronto iyo dhuxusha sida ilo kulaylka.
Marka laga hadlayo dhuxusha sida isha kulaylka, waxa ku jira AQ ayaa si aad ah u kordhay intii lagu jiray farsamaynta shaaha, oo kor u kacday 0.008 ilaa 0.038 mg/kg. 338.9% AQ ayaa lagu kordhiyey habka hagaajinta, gaarey 0.037 mg/kg, taas oo aad uga badan MRL ee 0.02 mg/kg oo ay dejisay Midowga Yurub. Inta lagu jiro marxaladda duubista, heerka AQ ayaa weli kordhay 5.8% inkastoo uu ka fog yahay mashiinka hagaajinta. Marka ugu horeysa ee la qalajiyo iyo dib-u-qallajinta, waxa ku jira AQ ayaa kordhay ama yara yaraatay. PF-yada u isticmaalaya dhuxusha sida isha kulaylka ee hagaajinta, qallajinta ugu horeysa iyo dib u qalajinta waxay ahaayeen 4.39, 1.05, 0.93, iyo 1.05, siday u kala horreeyaan.

Si loo sii go'aamiyo xidhiidhka ka dhexeeya gubashada dhuxusha iyo wasakhowga AQ, arrimaha la hakiyay (PMs) ee hawada ku jira aqoon-is-weydaarsiyada hoos yimaada labada ilo kulayl ayaa la ururiyay si loo qiimeeyo hawada, sida ku cad sawirka 4. Heerka AQ ee PM-yada leh dhuxusha sida Ilaha kulaylku wuxuu ahaa 2.98 μg/m3, kaas oo saddex jeer ka sarreeyay tan korontadu ahayd 0.91 μg/m3.

Jaantuska 4. Heerarka AQ ee deegaanka ee leh koronto iyo dhuxul sida isha kulaylka. * Waxay muujineysaa kala duwanaansho weyn oo heerarka AQ ee shaybaarada (p <0.05).

Heerarka AQ inta lagu jiro farsamaynta shaaha oolong shaaha Oolong, inta badan laga soo saaro Fujian iyo Taiwan, waa nooc ka mid ah shaaha qayb ahaan khamiirsan. Si loo sii go'aamiyo tillaabooyinka ugu muhiimsan ee kordhinta heerka AQ iyo saamaynta shidaalka kala duwan, isla dufcaddii caleemaha cusub ayaa laga dhigay shaaha oolong oo leh dhuxusha iyo gaaska-korontada dabiiciga ah sida ilo kulaylka, isku mar. Heerarka AQ ee diyaarinta shaaha oolong iyadoo la isticmaalayo ilo kulayl oo kala duwan ayaa lagu muujiyay sawirka 5. Si loo farsameeyo shaaha oolong ee leh gaaska-korontada dabiiciga ah, isbeddelka heerka AQ wuxuu ahaa mid fadhiid ah oo ka hooseeya 0.005 mg/kg, kaas oo la mid ah kan shaaha cagaaran koronto leh.

Jaantuska 5. Heerka AQ inta lagu jiro farsamaynta shaaha oolong oo leh gaaska-korontada dabiiciga ah iyo dhuxusha sida isha kulaylka.

Dhuxusha sida isha kulaylka, heerarka AQ ee labada tallaabo ee hore, engegay iyo samaynta cagaaran, waxay asal ahaan la mid ahaayeen isku dhafka gaaska-korontada ee dabiiciga ah. Si kastaba ha ahaatee, hababka xiga ilaa hagaajinta waxay muujiyeen farqiga u kordhay si tartiib tartiib ah, markaas oo heerka AQ uu kor u kacay 0.004 ilaa 0.023 mg / kg. Heerka tilaabada duubista ee xirxiran ayaa hoos u dhacday ilaa 0.018 mg/kg, taas oo ay sabab u tahay luminta casiirka shaaha oo qaaday qaar ka mid ah wasakhooyinka AQ. Marxaladda duubista ka dib, heerka heerka qalajinta ayaa kordhay ilaa 0.027 mg/kg. Marka engegan, samaynta cagaarka, hagaajinta, duuban iyo qalajinta, PF-yadu waxay ahaayeen 2.81, 1.32, 5.66, 0.78, iyo 1.50, siday u kala horreeyaan.

Dhacdada AQ ee alaabta shaaha ee leh ilo kulayl oo kala duwan

Si loo go'aamiyo saamaynta ay ku leedahay shaaha AQ ee leh ilo kulayl oo kala duwan, 40 muunado shaah ah oo laga soo qaaday aqoon-is-weydaarsiyada shaaha iyadoo la adeegsanayo koronto ama dhuxul sida ilaha kulaylka ayaa la falanqeeyay, sida ku cad Jadwalka 2. Marka la barbardhigo isticmaalka tamarta sida il kulaylka, dhuxusha ayaa ugu badan Heerarka baaritaanka (85.0%) oo leh heerka ugu sarreeya ee AQ ee 0.064 mg / kg, taas oo muujinaysa in ay fududahay in la keeno wasakhowga AQ ee qiiqa uu soo saaro gubashada dhuxusha, iyo heerka 35.0% ayaa lagu arkay muunadaha dhuxusha. Inta badan sida muuqata, korontadu waxay lahayd baarayaasha ugu hooseeya iyo heerarka sareynta ee 56.4% iyo 7.7% siday u kala horreeyaan, oo leh ugu badnaan 0.020 mg/kg.

DOOD

Iyada oo ku saleysan PF-yada inta lagu jiro farsamaynta labada nooc ee ilo kulaylka, way caddaatay in hagaajintu ay ahayd tillaabada ugu weyn ee keentay korodhka heerarka AQ ee wax soo saarka shaaha oo leh dhuxusha iyo ka shaqeynta tamarta korontada ayaa saameyn yar ku yeelatay nuxurka AQ shaaha ku jira. Inta lagu jiro farsamaynta shaaha cagaaran, gubashada dhuxusha waxay soo saartey qiiq badan habka hagaajinta marka la barbar dhigo habka kuleylka korontada, taas oo muujinaysa in laga yaabo in qiiqa uu ahaa isha ugu weyn ee wasakhowga AQ ee la xidhiidha caleemaha shaaha isla markiiba habka shaaha, oo la mid ah habka soo-gaadhista shaybaarada barbecue-ka ee la qiiqay[25]. Waxoogaa korodhka ah ee nuxurka AQ inta lagu guda jiro marxaladda duubista ayaa soo jeedisay in qiiqa ka dhasha gubashada dhuxusha aysan kaliya saameynin heerka AQ inta lagu jiro tallaabada hagaajinta, laakiin sidoo kale jawiga habaynta sababtoo ah kaydinta atmospheric. Dhuxusha ayaa sidoo kale loo isticmaalay sidii isha kulaylka marka ugu horeysa ee engejinta iyo dib-u-qallajinta, laakiin labadan tillaabo waxa ku jira AQ wax yar ayaa kordhay ama hoos u dhacay. Tan waxaa lagu macnayn karaa xaqiiqda ah in qalajiyaha dabayl kulul ee kuxiran uu shaaha ka fogeeyay qiiqa ka dhashay gubista dhuxusha[26]. Si loo go'aamiyo isha wasakhaysan, heerarka AQ ee jawiga ayaa la falanqeeyay, taasoo keentay farqi weyn oo u dhexeeya labada aqoon isweydaarsi. Sababta ugu weyn ee tan ayaa ah in dhuxusha loo isticmaalo hagaajinta, qalajinta ugu horeysa iyo marxaladaha dib u qalajinta ay dhalin doonto AQ inta lagu jiro gubasho aan dhamaystirnayn. AQ-yadan ayaa markaa lagu dhajiyay qaybo yaryar oo adag ka dib gubashada dhuxusha oo lagu kala firdhiyey hawada, taasoo kor u qaadeysa heerarka wasakhowga AQ ee jawiga aqoon-is-weydaarsiga[15]. Muddo ka dib, iyada oo ay ugu wacan tahay bedka weyn ee gaarka ah iyo awoodda shaaha, qaybahani waxay dageen dusha sare ee caleemaha shaaha, taasoo keentay kororka AQ ee wax soo saarka. Sidaa darteed, gubashada dhuxusha ayaa loo malaynayay inay tahay dariiqa ugu wayn ee keenaya wasakhaynta xad dhaafka ah ee AQ ee habaynta shaaha, iyadoo qiiqa uu yahay isha wasakhaysan.

Marka laga hadlayo farsamaynta shaaha oolong, AQ ayaa lagu kordhiyay iyada oo la adeegsanayo labada ilo kulaylka, laakiin farqiga u dhexeeya labada ilo kulaylka ayaa ahaa mid muhiim ah. Natiijooyinka ayaa sidoo kale soo jeediyay in dhuxusha sida isha kulaylka ay door weyn ka ciyaartay kordhinta heerka AQ, hagaajinta ayaa loo arkay inay tahay tallaabada ugu weyn ee kordhinta wasakheynta AQ ee diyaarinta shaaha oolong ee ku saleysan PF-yada. Intii lagu jiray farsamaynta shaaha oolong ee gaaska-korontada dabiiciga ah sida isha kulaylka, isbeddelka heerka AQ wuxuu ahaa mid ka hooseeya 0.005 mg/kg, kaas oo la mid ah kan shaaha cagaaran ee koronto, oo soo jeedinaya in tamarta nadiifka ah, sida korontada iyo dabiiciga ah. gaaska, waxa ay yarayn kartaa halista soo saarista wasakhaynta AQ ee ka shaqaynta.

Marka la eego shaybaarka, natiijadu waxay muujisay in xaaladda wasakhaysan ee AQ ay ka sii darnayd marka loo isticmaalo dhuxusha sida kulaylka halkii ay ka ahaan lahayd koronto, taas oo laga yaabo in ay sabab u tahay qiiqa gubanaya dhuxusha oo taabtay caleemaha shaaha oo ku raaga agagaarka goobta shaqada. Si kastaba ha ahaatee, in kasta oo ay iska caddahay in korontadu ay tahay isha kulaylka ugu nadiifsan inta lagu jiro habaynta shaaha, waxaa weli jiray wasakhowga AQ ee badeecadaha shaaha oo koronto ahaan u isticmaalaya isha kulaylka. Xaaladdu waxay u muuqataa wax yar oo la mid ah shaqo hore loo daabacay taas oo falcelinta 2-alkenals leh hydroquinones iyo benzoquinones loo soo jeediyay inay tahay dariiq kiimiko oo suurtagal ah[23], sababaha tan ayaa lagu baari doonaa cilmi-baarista mustaqbalka.

GUNAANAD

Shaqadan, ilaha suurtogalka ah ee wasakhowga AQ ee cagaarka iyo shaaha oolong ayaa lagu xaqiijiyay tijaabooyin isbarbardhig oo ku salaysan hababka falanqaynta ee GC-MS/MS ee la hagaajiyay. Natiijooyinkayagu waxay si toos ah u taageereen in isha ugu weyn ee wasakhaysan ee heerarka sare ee AQ ay tahay qiiq ka dhashay gubashada, taas oo aan saamaynaynin oo keliya marxaladaha habaynta laakiin sidoo kale saameeyay jawiga aqoon-is-weydaarsiga. Si ka duwan marxaladaha rogrogmada iyo engegan, halkaasoo isbeddellada heerka AQ ay ahaayeen kuwo aan muuqan, marxaladaha si toos ah ugu lug leh dhuxusha iyo xaabada, sida hagaajinta, waa habka ugu muhiimsan ee wasakhda AQ kor u kacday sababtoo ah qadarka xiriirka u dhexeeya shaaha. iyo qiiqa inta lagu jiro marxaladahan. Sidaa darteed, shidaal nadiif ah sida gaaska dabiiciga ah iyo korontada ayaa lagula taliyay inay yihiin isha kulaylka ee warshadaynta shaaha. Intaa waxaa dheer, natiijooyinka tijaabada ah ayaa sidoo kale muujiyay in maqnaanshaha qiiqa ka dhasha gubashada, ay jiraan arrimo kale oo gacan ka geysanaya raadinta AQ inta lagu jiro diyaarinta shaaha, halka xaddi yar oo AQ ah ayaa sidoo kale lagu arkay aqoon-is-weydaarsiga oo leh shidaal nadiif ah, taas oo ay tahay in baaritaan dheeraad ah lagu sameeyo. cilmi baarista mustaqbalka.

AALADAHA IYO HABKA

Reagents, kiimikooyin iyo agab

Heerka Anthraquinone (99.0%) waxaa laga soo iibsaday Dr. Ehrenstorfer GmbH Company (Augsburg, Germany). Heerka gudaha D8-Anthraquinone (98.6%) waxaa laga soo iibsaday C/D/N Isotopes (Quebec, Canada). Sulfate sodium anhydrous (Na2SO4) iyo magnesium sulfate (MgSO4) (Shanghai, Shiinaha). Florisil waxa siisay Wenzhou Organic Chemical Company (Wenzhou, Shiinaha). Warqadda fiber-ka-glass-ka ah (90 mm) waxaa laga soo iibsaday shirkadda Ahlstrom-munksjö (Helsingi, Finland).

Tusaalaha diyaarinta

Muunada shaaha cagaaran waxaa lagu farsameeyay hagaajin, rogrogid, qalajinta ugu horraysa iyo dib u qalajinta (iyadoo la isticmaalayo qalab ku lifaaqan), halka shaaha oolong laga soo saaray iyada oo engegan, laga dhigay cagaar (ruxan iyo caleemo cusub oo taagan si beddel ah), hagaajin, duub duuban, iyo qalajin. Tusaalooyinka tillaabo kasta ayaa la soo ururiyey saddex jeer 100g ka dib markii si fiican la isku qaso. Dhammaan shaybaarada waxaa lagu kaydiyay -20 °C si loo baaro.

Shaybaarada hawada waxaa lagu soo ururiyay warqad fiber galaas ah (90 mm) iyadoo la adeegsanayo muunad dhexdhexaad ah (PTS-100, Shirkadda Qingdao Laoshan Electronic Instrument Company, Qingdao, Shiinaha) [27], oo ku socota 100 L / min 4 h.

Tijaabooyin la xoojiyay ayaa lagu salaaxay AQ at 0.005 mg/kg, 0.010 mg/kg, 0.020 mg/kg ee caleemaha shaaha cusub, 0.005 mg/kg, 0.020 mg/kg, 0.050 mg/kg shaaha qalalan iyo 0.012 mg/kg (0.5 µg/m3 muunadda hawada), 0.036 mg/kg (1.5 µg/m3 hawo smaple), 0.072 mg/kg (3.0 µg/m3 ee muunad hawo) warqad filter galaas, siday u kala horreeyaan. Ka dib markaad si fiican u ruxdo, dhammaan shaybaarada ayaa laga tagay 12 saacadood, oo ay ku xigto soo saarista iyo nadiifinta.

Qoyaanka qoyaanka ah waxaa lagu helay qaadashada 20 g oo muunad ah ka dib marka la isku daro tillaabo kasta, kuleylinta 105 °C 1 saac, ka dibna miisaamaya oo ku celcelinaya saddex jeer oo qaadashada qiimaha celceliska iyo qaybinta miisaanka ka hor kuleylka.

Tusaalaha soo saarista iyo nadiifinta

Muunad shaaha: Soo saarista iyo nadiifinta AQ ee shaybaarada shaaha ayaa la sameeyay iyadoo lagu salaynayo habka la daabacay ee Wang et al. oo leh dhowr laqabsi[21]. Si kooban, 1.5 g oo muunado shaah ah ayaa marka hore lagu qasay 30 μL D8-AQ (2 mg/kg) waxaana loo daayay in ay istaagaan 30 min, ka dibna si fiican loogu qaso 1.5 mL biyo deionized oo loo daayay in ay istaagaan 30 min. 15 ml 20% acetone ee n-hexane ayaa lagu daray shaybaarka shaaha waxaana la soniced 15 min. Dabadeed shaybaarada waxaa lagu wareemay 1.0 g MgSO4 30 s, waxaana la saaray 5 min, 11,000 rpm. Ka dib markii loo raray 100 mL galaasyada qaabka pear-ka ah, 10 mL ee wajiga sare ee organic ayaa la uumi baxay ilaa ku dhawaad ​​qallayl hoostiisa 37 °C. 5 mL 2.5% acetone ee n-hexane ayaa dib u milantay soosaartii ku jirtay weel alwaax u eg si loo nadiifiyo. Tiirka galaaska (10 cm × 0.8 cm) wuxuu ka koobnaa hoos ilaa sare ee dhogor galaas ah iyo 2g florisil, kaas oo u dhexeeyay laba lakab oo 2 cm Na2SO4. Kadib 5 ml oo ah 2.5% acetone ee n-hexane ayaa horay u maydhay tiirka. Ka dib markii la raray xalka dib loo milmay, AQ ayaa saddex jeer lagu soo saaray 5 mL, 10 mL, 10 mL ee 2.5% acetone ee n-hexane. Eluates-ka la isku daray ayaa lagu wareejiyay weel u eg pear waxaana ay ku soo baxeen uumi ku dhawaad ​​qallayl hoostii vacuum 37 °C. Hadhaaga la qalajiyey ayaa markaa dib loogu dhisay 1 mL oo ah 2.5% acetone ee hexane oo ay ku xigto sifaynta iyada oo loo marayo shaandhaynta cabbirka daloolka 0.22 µm. Kadibna xalka dib loo dhisay ayaa lagu qasi jiray acetonitrile oo ah saamiga mugga 1: 1. Ka dib tillaabada gariirta, subnatant-ka waxa loo isticmaalay falanqaynta GC-MS/MS.

Muunadda hawada: Nus ka mid ah warqadda fiber-ka, oo lagu tiifay 18 μL d8-AQ (2 mg/kg), ayaa lagu dhex milmay 15 mL of 20% acetone ee n-hexane, ka dibna sonicated 15 min. Marxaladda dabiiciga ah waxaa lagu kala saaray centrifugation at 11,000 rpm 5 min iyo dhammaan lakabka sare ayaa laga saaray weel u eg pear. Dhammaan wejiyada organic-ga ah ayaa la uumi-baxay ilaa ku dhawaad ​​qallayl marka la nadiifiyo 37 °C. 5 ml oo ah 2.5% acetone oo hexane ah ayaa dib u milmaan kasaarkii sifaynta si la mid ah muunada shaaha.

Falanqaynta GC-MS/MS

Varian 450 gaas chromatograph oo ku qalabaysan Varian 300 tandem mass detector (Varian, Walnut Creek, CA, USA) ayaa loo isticmaalay in lagu sameeyo falanqaynta AQ iyada oo la adeegsanayo software MS WorkStation version 6.9.3. Factor Varian Afar tiir xidid VF-5ms (30m × 0.25 mm × 0.25 μm) ayaa loo isticmaalay kala soocida chromatographic. Gaaska xambaara, helium (> 99.999%), waxaa lagu dejiyay xadiga socodka joogtada ah ee 1.0 mL/min oo leh gaaska isku dhaca ee Argon (> 99.999%). Heerkulka foornada ayaa ka bilaabmay 80 ° C waxaana lagu hayaa 1 daqiiqo; wuxuu kordhay 15 °C/daqiiqo ilaa 240 °C, ka dibna wuxuu gaaray 260 °C at 20 °C/min waxaana lagu hayaa 5min. Heerkulka isha ion wuxuu ahaa 210 ° C, iyo sidoo kale heerkulka xariiqda wareejinta ee 280 ° C. Mugga duritaanku wuxuu ahaa 1.0 μL. Xaaladaha MRM waxaa lagu muujiyey shaxda 3.

Agilent 8890 chromatograph gaas oo ku qalabaysan Agilent 7000D triple quadrupole mass spectrometer (Agilent, Stevens Creek, CA, USA) ayaa loo isticmaalay in lagu falanqeeyo saamaynta sifaynta ee nooca MassHunter 10.1 software. Agilent J&W HP-5ms GC Column (30m × 0.25 mm × 0.25 μm) ayaa loo isticmaalay kala soocida chromatographic. Gaaska xambaara, Helium (> 99.999%), waxaa lagu dejiyay xadiga socodka joogtada ah ee 2.25 mL/min oo leh gaaska isku dhaca ee Nitrogen (> 99.999%). Heerkulka isha EI ion waxaa lagu hagaajiyay 280 °C, oo la mid ah heerkulka xariiqda wareejinta. Heerkulka foornada ayaa ka bilaabmay 80 ° C waxaana lagu hayaa 5 min; kor loo qaaday 15 °C/daqiiqo ilaa 240 °C, ka dibna la gaarey 280 °C at 25 °C/min waxaana lagu hayaa 5 daqiiqo. Xaaladaha MRM waxaa lagu muujiyey shaxda 3.

Falanqaynta tirakoobka
Nuxurka AQ ee caleemaha cusub waxaa lagu saxay nuxurka walxaha qalalan iyadoo loo qaybinayo qoyaanka si loo barbardhigo loona falanqeeyo heerarka AQ inta lagu jiro habaynta.

Isbeddellada AQ ee muunadaha shaaha waxaa lagu qiimeeyay Microsoft Excel software iyo IBM SPSS Statistics 20.

Qodobka habaynta ayaa loo isticmaalay in lagu qeexo isbeddelada AQ inta lagu jiro habaynta shaaha. PF = Rl/Rf , halka Rf uu yahay heerka AQ ka hor inta aan la qaadin tilaabada habaynta iyo Rl waa heerka AQ ka dib talaabada habaynta. PF waxay muujinaysaa hoos u dhac (PF <1) ama korodhka (PF> 1) ee hadhaaga AQ inta lagu jiro tallaabo habaysan oo gaar ah.

ME waxay muujineysaa hoos u dhac (ME <1) ama koror (ME> 1) iyada oo laga jawaabayo aaladaha falanqaynta, taas oo ku saleysan saamiga jiirada jaangooyooyinka ee shaxanka iyo dareeraha sida soo socota:

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

Meesha slopematrix ay tahay jiirada qalooca calibration ee dareeraha matrix-ku-ku-maaxsan, slopesolvent waa jiirada qalooca calibration ee dareeraha.

MAHADSANID
Shaqadan waxaa taageeray Sayniska iyo Tignoolajiyada Mashruuca Weyn ee Gobolka Zhejiang (2015C12001) iyo Aasaaska Sayniska Qaranka ee Shiinaha (42007354).
Iska hor imaadka danaha
Qorayaashu waxay caddeeyeen in aanay lahayn iska hor imaad daneed.
Xuquuqda iyo ogolaanshaha
Xuquuqda daabacaada: © 2022 waxaa leh qoraaga(-yaasha). Shatiga Gaarka ah ee ugu sarreeya saxaafadda, Fayetteville, GA. Maqaalkani waa maqaal gelitaan furan oo lagu qaybiyay shatiga Astaanta Hal-abuurka Guud (CC BY 4.0), booqo https://creativecommons.org/licenses/by/4.0/.
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Ku saabsan maqaalkan
Xigasho maqaalkan
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