Abstract
9,10-Anthraquinone (AQ) bụ ihe na-efe efe nwere ihe ize ndụ nke carcinogenic ma na-eme na tii n'ụwa nile. Oke kacha nke fọdụrụ (MRL) nke AQ na tii nke European Union (EU) setịpụrụ bụ 0.02 mg/kg. A nyochara isi mmalite nke AQ na nhazi tii na isi ihe mere ya dabere na usoro nyocha AQ gbanwere yana nyocha gas chromatography-tandem mass spectrometry (GC-MS/MS). E jiri ya tụnyere ọkụ eletrik dị ka isi iyi ọkụ na nhazi tii green, AQ mụbara site na 4.3 ruo 23.9 ugboro na nhazi tii na coal dị ka isi iyi ọkụ, karịrị 0.02 mg / kg, ebe ọkwa AQ dị na gburugburu ebe obibi okpukpu atọ. A hụrụ otu ihe a na-eme na nhazi tii oolong n'okpuru ọkụ coal. A na-ewere usoro ndị nwere kọntaktị kpọmkwem n'etiti akwụkwọ tii na uzuzu, dị ka nhazi na ihicha, dịka isi nzọụkwụ nke mmepụta AQ na nhazi tii. Ọkwa AQ mụbara na oge kọntaktị na-arị elu, na-atụ aro na ọkwa dị elu nke mmetọ AQ na tii nwere ike nweta site na uzuzu nke coal na combustion kpatara. Ihe nlele iri anọ sitere na ụlọ ọrụ dị iche iche nwere ọkụ eletrik ma ọ bụ coal ka a na-enyocha isi mmalite okpomọkụ, sitere na 50.0% -85.0% na 5.0% -35.0% maka nchọpụta na gafere ọnụego AQ. Tụkwasị na nke ahụ, a na-ahụ ihe kachasị AQ nke 0.064 mg / kg na ngwaahịa tii na coal dị ka isi iyi ọkụ, na-egosi na oke ọkwa nke AQ na-emerụ emerụ na ngwaahịa tii nwere ike inye aka site na coal.
Keywords: 9,10-Anthraquinone, Nhazi tii, Coal, isi iyi mmetọ
Okwu mmalite
Tii emepụtara site na epupụta nke osisi shrub mgbe ọ bụla Camellia sinensis (L.) O. Kuntze, bụ otu n'ime ihe ọṅụṅụ na-ewu ewu n'ụwa nile n'ihi uto na-enye ume ọhụrụ na uru ahụike. Na 2020 n'ụwa niile, mmepụta tii abawanyela ruo nde metric ton 5,972, nke bụ okpukpu abụọ n'ime afọ 20 gara aga[1]. Dabere na ụzọ dị iche iche isi edozi isi, enwere ụdị tii isii, gụnyere tii tii, tii ojii, tii gbara ọchịchịrị, tii oolong, tii ọcha na tii odo[2,3]. Iji hụ na ịdị mma na nchekwa nke ngwaahịa, ọ dị ezigbo mkpa iji nyochaa ọkwa nke mmetọ ma kọwaa mmalite.

Ịmata isi mmalite nke mmetọ, dị ka ihe fọdụrụ na pesticide, ọla arọ na mmetọ ndị ọzọ dị ka polycyclic aromatic hydrocarbons (PAHs), bụ nzọụkwụ mbụ iji chịkwaa mmetọ. Ịfesa kemịkalụ sịntetik ozugbo n'ugbo tii, yana ịfefe ikuku nke arụrụ n'akụkụ ogige tii na-ebute bụ isi ebe a na-enweta nsị pesticide na tii[4]. Ọla dị arọ nwere ike ịgbakọta na tii wee bute nsị, bụ nke sitere na ala, fatịlaịza na ikuku [5-7]. N'ihe gbasara mmetọ ndị ọzọ na-apụta na tii na-atụghị anya ya, ọ bụ ihe siri ike ịmata n'ihi usoro mgbagwoju anya nke mmepụta tii tii gụnyere ihe ọkụkụ, nhazi, ngwugwu, nchekwa na njem. Ndị PAH dị na tii sitere n'ịkwakọba iyuzucha ụgbọ ala na ọkụ ọkụ a na-eji n'oge nhazi akwụkwọ tii, dị ka nkụ na kol[8-10].

N'oge a na-agba ọkụ na coal na nkụ, a na-emepụta ihe ndị na-emetọ ihe dị ka carbon oxides[11]. N'ihi ya, ọ na-adị mfe ka ihe ndị a na-emetọ ihe ndị a e kwuru n'elu na-eme na ngwaahịa ndị a na-emepụta, dị ka ọka, ngwaahịa a na-ese anwụrụ na azụ nwamba, na okpomọkụ dị elu, na-etinye ihe ize ndụ nye ahụike mmadụ[12,13]. A na-enweta PAH ndị sitere na combustion site na ngbanwe nke PAH dị na mmanụ ọkụ n'onwe ya, nrụrụ okpomọkụ dị elu nke ogige aromatic na mmeghachi omume n'etiti free radicals[14]. Okpomọkụ ọkụ, oge, na ikuku oxygen bụ ihe dị mkpa na-emetụta mgbanwe nke PAH. Site na mmụba nke okpomọkụ, ọdịnaya PAH buru ụzọ mụbaa wee belata, ọnụ ahịa kachasị elu mere na 800 Celsius; Ọdịnaya PAH gbadara nke ọma iji chọpụta na oge ọkụ ọkụ na-abawanye mgbe ọ nọ n'okpuru oke a na-akpọ 'oge oke', yana mmụba nke ọdịnaya oxygen na ikuku combustion, ikuku PAH na-ebelata nke ukwuu, mana oxidation na-ezughị ezu ga-emepụta OPAHs na ihe ndị ọzọ[15]. -17].

9,10-Anthraquinone (AQ, CAS: 84-65-1, Fig. 1), ihe na-emepụta oxygen-nwere nke PAHs [18], nwere usoro mgbagwoju anya atọ. Edepụtara ya dị ka ọrịa carcinogen (Group 2B) nke International Agency for Research on Cancer na 2014[19]. AQ nwere ike imebi topoisomerase II cleavage complex ma gbochie hydrolysis nke adenosine triphosphate (ATP) site na DNA topoisomerase II, na-eme ka DNA okpukpu abụọ gbajie, nke pụtara na ikpughe ogologo oge n'okpuru AQ nwere gburugburu ebe obibi na kọntaktị kpọmkwem na ọkwa dị elu nke AQ. nwere ike ibute mmebi DNA, mmụgharị na ịbawanye ohere nke ọrịa kansa[20]. Dị ka mmetụta na-adịghị mma na ahụ ike mmadụ, oke AQ kachasị mma (MRL) nke 0.02 mg/kg ka European Union setịpụrụ na tii. Dị ka ọmụmụ anyị gara aga si kwuo, a na-atụ aro nkwụnye ego nke AQ dị ka isi mmalite n'oge ịkụ tii[21]. Ọzọkwa, dabere na nnwale nnwale na Indonesian green na black tii nhazi, o doro anya na ọkwa AQ gbanwere nke ukwuu na anwụrụ ọkụ sitere na ngwa nhazi bụ otu n'ime isi ihe kpatara ya [22]. Otú ọ dị, ezi mmalite nke AQ na nhazi tii nọgidere bụrụ ihe siri ike, ọ bụ ezie na a tụrụ aro ụfọdụ echiche nke ụzọ kemịkalụ AQ[23,24], na-egosi na ọ dị oke mkpa iji chọpụta ihe ndị dị mkpa na-emetụta ọkwa AQ na nhazi tii.

Ọgụgụ 1. Usoro kemịkalụ nke AQ.

N'iburu nyocha banyere nguzobe AQ n'oge combustion coal na ihe ize ndụ nke mmanụ ọkụ na nhazi tii, e mere nnwale atụnyere iji kọwaa mmetụta nke nhazi isi mmalite okpomọkụ na AQ na tii na ikuku, nyocha ọnụọgụ na mgbanwe nke ọdịnaya AQ. na usoro nhazi dị iche iche, nke na-enye aka iji kwado mmalite ziri ezi, ụkpụrụ omume na ogo nke mmetọ AQ na nhazi tii.

Nsonaazụ
Nkwenye usoro
E jiri ya tụnyere ọmụmụ ihe anyị gara aga[21], a na-ejikọta usoro mmịpụta mmiri mmiri tupu ịgbanye GC-MS/MS iji mee ka uche dịkwuo mma ma nọgide na-enwe nkwupụta ngwá ọrụ. Na Fig 2b, usoro a na-emeziwanye gosipụtara ọganihu dị ukwuu na nchacha nke ihe nlele ahụ, ihe mgbaze ahụ ghọrọ ọkụ na agba. Na Fig 2a, ụdị nyocha zuru oke (50-350 m / z) gosipụtara na mgbe emechara ọcha, akara ntọala nke ụdị MS dị iche iche belatara n'ụzọ doro anya na ọnụ ọgụgụ chromatographic dị ole na ole dị, na-egosi na e wepụrụ ọnụ ọgụgụ buru ibu nke ogige nnyonye anya mgbe nke ahụ gasịrị. mmịpụta mmiri mmiri.

Ọgụgụ 2. (a) Nleba anya zuru oke nke nlele tupu na mgbe emechara ọcha. (b) Mmetụta dị ọcha nke usoro emelitere.
Nkwenye usoro, gụnyere linearity, mgbake, njedebe nke quntitation (LOQ) na mmetụta matrix (ME), na-egosi na Tebụl 1. Ọ na-enye afọ ojuju iji nweta linearity na ọnụọgụ nke mkpebi (r2) dị elu karịa 0.998, nke sitere na 0.005. na 0.2 mg / kg na tii matrix na acetonitrile mgbaze, na n'ikuku sample na nso nke 0,5 ka 8 μg / m3.

A tụlere mgbake nke AQ na mkpokọta spiked atọ dị n'etiti nha nha na n'ezie na tii akọrọ (0.005, 0.02, 0.05 mg / kg), ome tii ọhụrụ (0.005, 0.01, 0.02 mg / kg) na nlele ikuku (0.5, 1.5, 3). μg/m3). Iweghachite AQ na tii sitere na 77.78% ruo 113.02% na tii akọrọ yana site na 96.52% ruo 125.69% na tii tii, yana RSD% dị ala karịa 15%. Iweghachite AQ na nlele ikuku sitere na 78.47% ruo 117.06% yana RSD% n'okpuru 20%. Achọpụtara mkpokọta kachasị dị ala dị ka LOQ, nke bụ 0.005 mg/kg, 0.005 mg/kg na 0.5 μg/m³ na ome tii, tii akọrọ na ihe nlele ikuku, n'otu n'otu. Dị ka e depụtara na Tebụl 1, matrix nke tii akọrọ na tii tii mụbara nzaghachi AQ, na-eduga na ME nke 109.0% na 110.9%. Banyere matriks nke ihe nlele ikuku, ME bụ 196.1%.

The ọkwa nke AQ n'oge green tii nhazi
N'ebumnuche nke ịchọpụta mmetụta dị iche iche dị iche iche na-ekpo ọkụ na tii na nhazi gburugburu ebe obibi, a na-ekewa batch nke akwụkwọ ọhụrụ n'ime otu abụọ ma hazie ya iche na ụlọ ọrụ nhazi abụọ n'otu ụlọ ọrụ. E nyere otu ìgwè ọkụ eletrik, nke ọzọ na-ebukwa coal.

Dị ka e gosiri na Fig. 3, ọkwa AQ na ọkụ eletrik dị ka isi iyi ọkụ sitere na 0.008 ruo 0.013 mg / kg. N'oge usoro nhazi ahụ, ịhịa aka n'ahụ nke akwụkwọ tii mere site na nhazi n'ime ite nwere okpomọkụ dị elu mere ka mmụba 9.5% dị na AQ. Mgbe ahụ, ọkwa AQ nọgidere n'oge usoro ntụgharị n'agbanyeghị nkwụsị nke ihe ọṅụṅụ, na-atụ aro na usoro anụ ahụ nwere ike ọ gaghị emetụta ọkwa AQ na nhazi tii. Mgbe usoro ihicha nke mbụ gasịrị, ọkwa AQ mụbara ntakịrị site na 0.010 ruo 0.012 mg / kg, wee gaa n'ihu na-arị elu ruo 0.013 mg / kg ruo mgbe njedebe nke ihicha ọzọ. PF, nke gosipụtara n'ụzọ doro anya mgbanwe dị na nzọụkwụ ọ bụla, bụ 1.10, 1.03, 1.24, 1.08 na nhazi, ntụgharị, ihicha mbụ na ihicha ọzọ, n'otu n'otu. Nsonaazụ nke PF na-atụ aro na nhazi n'okpuru ike eletrik nwere mmetụta dị nta na ọkwa AQ na tii.

Ọgụgụ 3. Ọkwa AQ n'oge nhazi tii green na ọkụ eletrik na kol dị ka isi mmalite okpomọkụ.
N'ihe banyere coal dị ka isi iyi ọkụ, ọdịnaya AQ mụbara nke ukwuu n'oge nhazi tii, na-esi na 0.008 ruo 0.038 mg / kg. 338.9% AQ na-abawanye na usoro nhazi, na-eru 0.037 mg / kg, nke karịrị MRL nke 0.02 mg / kg nke European Union setịpụrụ. N'oge a na-atụgharị, ọkwa AQ ka na-abawanye site na 5.8% n'agbanyeghị na ọ dị anya site na igwe ndozi. Na ihicha mbụ na ihicha ọzọ, ọdịnaya AQ mụbara ntakịrị ma ọ bụ belata ntakịrị. Ndị PF na-eji coal dị ka isi iyi ọkụ na ndozi, na-atụgharị ihicha mbụ na ihicha ọzọ bụ 4.39, 1.05, 0.93, na 1.05, n'otu n'otu.

Iji chọpụtakwuo mmekọrịta dị n'etiti coal combustion na AQ mmetọ, ndị kwụsịtụrụ particulate okwu (PMs) na ikuku na ogbako n'okpuru ma okpomọkụ isi iyi ka anakọtara maka ikuku ntule, dị ka e gosiri na Fig. 4. The AQ larịị PMs na coal dị ka. isi iyi ọkụ bụ 2.98 μg / m3, nke karịrị okpukpu atọ karịa nke ọkụ eletrik 0.91 μg / m3.

Ọgụgụ 4. Ọkwa AQ na gburugburu ebe obibi na ọkụ eletrik na kol dị ka isi iyi ọkụ. * Na-egosi ọdịiche dị ukwuu na ọkwa AQ na nlele (p <0.05).

Ọkwa AQ n'oge a na-edozi tii oolong Oolong tii, nke emebere na Fujian na Taiwan, bụ ụdị tii nwere akụkụ fermented. Iji chọpụta n'ihu na isi nzọụkwụ nke ịba ụba AQ larịị na mmetụta nke dị iche iche mmanụ ụgbọala, otu ogbe nke ọhụrụ epupụta e mere na oolong tii na coal na eke gas-electric ngwakọ dị ka okpomọkụ isi mmalite, n'out oge. A na-egosi ọkwa AQ na nhazi tii oolong site na iji isi mmalite okpomọkụ dị iche iche na Fig. 5. Maka nhazi tii oolong na gas-electric hybrid, usoro nke ọkwa AQ na-adaba n'okpuru 0.005 mg / kg, nke yiri nke ahụ na tii green. na ọkụ eletrik.

Ọgụgụ 5. Ọkwa AQ n'oge nhazi tii oolong na ngwakọta gas-eletrik na coal dị ka isi iyi ọkụ.

Site na coal dị ka isi iyi ọkụ, ọkwa AQ na nzọụkwụ abụọ mbụ, akpọnwụ ma na-eme akwụkwọ ndụ akwụkwọ ndụ, bụ otu ihe ahụ na ngwakọta gas-eletrik. Otú ọ dị, usoro ndị na-esote ruo mgbe nhazi gosipụtara ọdịiche ahụ ji nwayọọ nwayọọ gbasaa, ebe ọkwa AQ si na 0.004 ruo 0.023 mg / kg. Ọkwa dị na ngwungwu ngwungwu ngagharị gbadara ruo 0.018 mg/kg, nke nwere ike ịbụ n'ihi mfu nke ihe ọṅụṅụ tii na-ebupụ ụfọdụ ihe mmetọ AQ. Mgbe usoro ntụgharị ahụ gasịrị, ọkwa dị na ihicha ahụ mụbara ruo 0.027 mg / kg. N'ịkpọnwụ, na-eme akwụkwọ ndụ akwụkwọ ndụ, ndozi, mkpọkọ mpịakọta na ihicha, PF bụ 2.81, 1.32, 5.66, 0.78, na 1.50, n'otu n'otu.

Ihe omume AQ na ngwaahịa tii nwere isi mmalite okpomọkụ dị iche iche

Iji chọpụta mmetụta dị na ọdịnaya AQ nke tii dị iche iche na-ekpo ọkụ, 40 tii samples sitere na ụlọ ọrụ tii na-eji ọkụ eletrik ma ọ bụ coal ka a na-enyocha ihe ndị na-ekpo ọkụ, dị ka e gosiri na Tebụl 2. N'iji ya tụnyere iji ọkụ eletrik dị ka isi iyi ọkụ, coal nwere ihe kachasị. Ọnụ ọgụgụ nchọpụta (85.0%) na ọkwa AQ kachasị elu nke 0.064 mg / kg, na-egosi na ọ dị mfe ime ka AQ na-emerụ ahụ site na uzuzu nke ọkụ ọkụ na-emepụta, na ọnụ ọgụgụ nke 35.0% hụrụ na nlele nke coal. Ọtụtụ n'ụzọ pụtara ìhè, ọkụ eletrik nwere ihe nchọpụta kachasị dị ala na nke kachasị elu nke 56.4% na 7.7% n'otu n'otu, yana ọdịnaya kachasị nke 0.020 mg / kg.

Mkparịta ụka

Dabere na PF n'oge nhazi ya na ụdị ọkụ ọkụ abụọ ahụ, o doro anya na nhazi bụ isi ihe kpatara mmụba nke ọkwa AQ na mmepụta tii na coal na nhazi n'okpuru ike eletrik nwere mmetụta dị nta na ọdịnaya nke AQ. na tii. N'oge nhazi akwụkwọ ndụ akwụkwọ ndụ tii, ọkụ ọkụ na-emepụta ọtụtụ uzuzu na nhazi nhazi ma e jiri ya tụnyere usoro ọkụ ọkụ eletrik, na-egosi na ma eleghị anya uzuzu bụ isi ihe na-emetọ AQ site na kọntaktị na tii tii ozugbo na nhazi tii, yiri usoro ikpughe na. sample barbecue a na-ese anwụrụ[25]. Mmụba dị ntakịrị na ọdịnaya AQ n'oge a na-atụgharị na-atụ aro na uzu ọkụ nke ọkụ ọkụ na-eme ka ọ bụghị nanị na-emetụta ọkwa AQ n'oge nhazi nhazi, kamakwa na gburugburu ebe nhazi n'ihi ntinye ikuku. A na-ejikwa coals mee ihe dị ka isi iyi ọkụ na ihicha mbụ na ihicha ọzọ, ma n'ime usoro abụọ a, ọdịnaya AQ mụbara ntakịrị ma ọ bụ belata ntakịrị. Enwere ike ịkọwa nke a site na eziokwu ahụ bụ na igwe nkụ nke ikuku na-ekpo ọkụ na-egbochi tii pụọ na uzuzu nke combustion coal kpatara[26]. Iji chọpụta isi iyi na-emetọ ihe, a na-enyocha ọkwa AQ dị na mbara igwe, na-ebute nnukwu ọdịiche dị n'etiti ụlọ ọrụ abụọ ahụ. Isi ihe kpatara nke a bụ na coal a na-eji na-edozi, nke mbụ ihicha na nhazigharị ga-emepụta AQ n'oge ọkụ na-ezughị ezu. A na-etinye AQ ndị a n'ime obere akụkụ nke ihe siri ike mgbe ọkụ kol gbasasịa na ikuku, na-ebuli ọkwa nke mmetọ AQ na gburugburu ebe ogbako [15]. Ka oge na-aga, n'ihi nnukwu ebe dị elu na ikike adsorption nke tii, ihe ndị a na-edozi n'elu akwụkwọ tii, na-ebute mmụba nke AQ na mmepụta. Ya mere, a na-eche na ikpo ọkụ coal bụ ụzọ bụ isi na-eduga n'oke mmetọ AQ na nhazi tii, na uzuzu bụ isi iyi nke mmetọ.

Banyere nhazi tii oolong, AQ na-abawanye n'okpuru nhazi ya na isi mmalite okpomọkụ, mana ọdịiche dị n'etiti isi mmalite okpomọkụ abụọ dị ịrịba ama. Nsonaazụ ahụ tụkwara aro na coal dị ka isi iyi ọkụ na-ekere òkè dị ukwuu n'ịbawanye ọkwa AQ, a na-ahụkwa nrụzi ahụ dị ka isi nzọụkwụ maka ịbawanye mmetọ AQ na nhazi tii oolong dabere na PF. N'oge nhazi tii oolong na ngwakọ gas-eletrik dị ka isi iyi ọkụ, usoro nke ọkwa AQ nọ na-agbada n'okpuru 0.005 mg / kg, nke yiri nke na tii green na ọkụ eletrik, na-atụ aro na ike dị ọcha, dị ka ọkụ eletrik na eke. gas, nwere ike ibelata ihe ize ndụ nke imepụta mmetọ AQ site na nhazi.

N'ihe gbasara nyocha nlele, nsonaazụ gosipụtara na ọnọdụ nke mmetọ AQ dị njọ mgbe ị na-eji coal dị ka ọkụ ọkụ karịa ọkụ eletrik, nke nwere ike ịbụ n'ihi uzuzu sitere na combustion nke coal na-abata na kọntaktị tii tii ma na-adịgide adịgide n'ebe ọrụ. Otú ọ dị, ọ bụ ezie na o doro anya na ọkụ eletrik bụ ebe okpomọkụ kachasị dị ọcha n'oge nhazi tii, a ka nwere AQ na-emerụ emerụ na ngwaahịa tii na-eji ọkụ eletrik dị ka isi iyi ọkụ. Ọnọdụ ahụ yiri ka ọ dị ntakịrị ka ọrụ e bipụtara na mbụ nke mmeghachi omume nke 2-alkenals na hydroquinones na benzoquinones tụrụ aro dị ka ụzọ kemịkalụ nwere ike[23], a ga-enyocha ihe kpatara nke a na nyocha n'ọdịnihu.

NKWUBIOKWU

N'ime ọrụ a, enwetara isi mmalite nke mmetọ AQ na akwụkwọ ndụ akwụkwọ ndụ na tii oolong site na nnwale atụnyere dabere na usoro nyocha GC-MS/MS emelitere. Nchọpụta anyị kwadoro ozugbo na isi iyi na-emetọ ihe dị elu nke AQ bụ uzuzu nke ọkụ ọkụ kpatara, nke na-abụghị nanị na-emetụta usoro nhazi kamakwa na-emetụta gburugburu ebe ọmụmụ ihe. N'adịghị ka n'ọkpụkpụ na-agbagharị ma na-akpọnwụ, ebe mgbanwe na ọkwa AQ na-apụtaghị ìhè, usoro ndị na-etinye aka kpọmkwem na coal na nkụ, dị ka nhazi, bụ usoro bụ isi nke mmetọ AQ bilitere n'ihi ọnụ ọgụgụ nke kọntaktị dị n'etiti tii. na uzuoku n'oge usoro ndị a. Ya mere, a na-atụ aro mmanụ ọkụ dị ọcha dị ka gas na ọkụ eletrik dị ka isi iyi ọkụ na nhazi tii. Na mgbakwunye, nsonaazụ nnwale ahụ gosikwara na na enweghị uzuoku sitere na combustion, a ka nwere ihe ndị ọzọ na-enye aka na-achọpụta AQ n'oge nhazi tii, ebe a na-ahụkwa obere AQ na ogbako ahụ nwere mmanụ ọkụ dị ọcha, nke kwesịrị inyochakwu nyocha. na nyocha n'ọdịnihu.

AKỤRỤNGWA NA ỤZỌ

Reagents, kemịkalụ na ihe

A zụrụ ọkọlọtọ Anthraquinone (99.0%) n'aka Dr. Ehrenstorfer GmbH Company (Augsburg, Germany). A zụtara ọkọlọtọ ime D8-Anthraquinone (98.6%) site na C/D/N Isotopes (Quebec, Canada). Anhydrous sodium sulfate (Na2SO4) na magnesium sulfate (MgSO4) (Shanghai, China). Wenzhou Organic Chemical Company (Wenzhou, China) wetara Florisil. Azụtara akwụkwọ fiber Mircro-glass (90 mm) n'aka ụlọ ọrụ Ahlstrom-munksjö (Helsinki, Finland).

Nkwadebe ihe atụ

A na-edozi ihe nlele tii akwụkwọ ndụ akwụkwọ ndụ site na nhazi, ntụgharị, ihicha mbụ na ihicha ọzọ (iji ngwá ọrụ mechiri emechi), ebe a na-edozi sample tii oolong na nkụ, na-eme akwụkwọ ndụ akwụkwọ ndụ (na-ama jijiji ma na-eguzo ọtọ ọzọ), nhazi, na-atụgharị, na ihicha. A na-anakọta ihe nlele site na nzọụkwụ ọ bụla ugboro atọ na 100g mgbe agwakọtachara nke ọma. A na-echekwa ihe nlele niile na -20 Celsius maka nyocha ọzọ.

A na-anakọta ihe nlele ikuku site na akwụkwọ eriri iko (90 mm) na-eji ndị na-eme ihe na-ajụkarị (PTS-100, Qingdao Laoshan Electronic Instrument Company, Qingdao, China) [27], na-agba ọsọ na 100 L / min maka 4 h.

A na-eji AQ mee ihe na 0.005 mg / kg, 0.010 mg / kg, 0.020 mg / kg maka ome tii ọhụrụ, na 0.005 mg / kg, 0.020 mg / kg, 0.050 mg / kg maka tii akọrọ na 0.012 mg / kg. (0.5 μg / m3 maka nlele ikuku), 0.036 mg / kg (1.5 µg / m3 maka ikuku smaple), 0.072 mg / kg (3.0 μg / m3 maka nlele ikuku) maka akwụkwọ nzacha iko, n'otu n'otu. Mgbe emechara nke ọma, a na-ahapụ ihe nlele niile maka awa 12, na-esote mmịpụta na usoro nhicha.

A na-enweta mmiri mmiri ahụ site n'inweta 20 g nke ihe nlele mgbe ọ gwakọtara nzọụkwụ ọ bụla, na-ekpo ọkụ na 105 Celsius maka 1 h, wee tụọ ma na-emegharị ugboro atọ ma na-ewere nkezi uru ma kewaa ya site na ibu tupu ikpo ọkụ.

Nlereanya mmịpụta na nhichapụ

Nlele tii: Mwepụta na ịdị ọcha nke AQ sitere na nlele tii ka emere dabere na usoro ebipụtara sitere na Wang et al. nwere ọtụtụ mgbanwe[21]. Na nkenke, a na-agwakọta 1.5 g nke ihe atụ tii na 30 μL D8-AQ (2 mg / kg) wee hapụ ka ọ kwụrụ maka 30 min, wee gwakọta ya na 1.5 mL mmiri deionized nke ọma wee hapụ ka ọ kwụrụ maka 30 min. 15 mL 20% acetone na n-hexane ka agbakwunyere na tii sample na sonicated maka 15 min. Mgbe ahụ, ejiri 1.0 g MgSO4 vortexed ihe atụ ndị ahụ maka 30 s, na centrifuged maka 5 min, na 11,000 rpm. Mgbe ebufere ya na 100 ml nke flask nke yiri ube, 10 ml nke akụkụ ahụ nke elu na-ekpochapụ ka ọ bụrụ nkụ n'okpuru oghere na 37 Celsius. 5 ml 2.5% acetone na n-hexane gbazekwara mwepu ahụ n'ime flask ndị nwere ụdị ube maka ịdị ọcha. Ogidi iko (10 cm × 0.8 cm) sitere na ala ruo n'elu nke ajị iko na 2g florisil, nke dị n'etiti akwa abụọ nke 2 cm Na2SO4. Mgbe ahụ, 5 ml nke 2.5% acetone na n-hexane sachachara kọlụm ahụ. Mgbe o kwusịrị ihe ngwọta agbazere, AQ ji 5 ml, 10 ml, 10 ml nke 2.5% acetone na n-hexane gbapụta ugboro atọ. Ebufere eluates ndị a jikọtara na flask ndị yiri ube wee kpochaa ruo ihe fọrọ nke nta ka ọ bụrụ nkụ n'okpuru oghere na 37 Celsius. Ejiri 1 mL nke 2.5% acetone na hexane wee megharịa ihe fọdụrụ akpọnwụ akpọnwụ site na nzacha nha nha 0.22µm. Mgbe ahụ, a na-agwakọta ihe ngwọta edozigharịrị na acetonitrile na oke olu nke 1: 1. Na-eso usoro ịma jijiji ahụ, ejiri subnatant mee nyocha GC-MS/MS.

Ihe nlele ikuku: Ọkara nke akwụkwọ eriri, nke 18 μL d8-AQ (2 mg / kg) gbanyere n'ime 15 mL nke 20% acetone na n-hexane, wee sonicated maka 15 min. A na-ekewa usoro organic site na centrifugation na 11,000 rpm maka 5 min ma wepụ ihe niile dị elu n'ime flask yiri ube. A na-ekpochapụ akụkụ niile nke organic ka ọ fọrọ nke nta ka ọ bụrụ nkụ n'okpuru oghere na 37 Celsius. 5 ml nke 2.5% acetone na hexane gbazere ihe ndị ahụ maka ịdị ọcha n'otu ụzọ ahụ dị na nlele tii.

Nyocha GC-MS/MS

Varian 450 gas chromatograph nke nwere Varian 300 tandem mass detector (Varian, Walnut Creek, CA, USA) ka ejiri mee nyocha AQ na ụdị MS WorkStation 6.9.3 software. Isi ihe dị iche iche ejirila kọlụm capillary anọ VF-5ms (30 m × 0.25 mm × 0.25 μm) maka nkewa chromatographic. The ebu gas, helium (> 99.999%), atọrọ na a na-aga n'ihu na-erute ọnụego nke 1.0 mL / min na nkukota gas nke Argon (> 99.999%). Okpomọkụ oven malitere site na 80 Celsius C wee jide 1 min; mụbara na 15 Celsius C / min ruo 240 Celsius C, wee ruo 260 Celsius C na 20 Celsius C / min wee jide 5min. Okpomọkụ nke isi iyi ion bụ 210 Celsius C, yana okpomoku ahịrị mbufe nke 280 Celsius. Olu injection bụ 1.0 μl. Egosiri ọnọdụ MRM na Tebụl 3.

Agilent 8890 gas chromatograph nke nwere Agilent 7000D triple quadrupole mass spectrometer (Agilent, Stevens Creek, CA, USA) ejirila ngwanrọ MassHunter 10.1 nyochaa mmetụta ịdị ọcha. Agilent J&W HP-5ms GC Kọlụm (30m × 0.25 mm × 0.25 μm) ka ejiri maka nkewa chromatographic. The ebu gas, Helium (> 99.999%), ka edobere na ọsọ ọsọ nke 2.25 mL / min na ikuku nkukota nke Nitrogen (> 99.999%). A na-edozi ọnọdụ okpomọkụ nke isi iyi EI na 280 Celsius C, otu ihe ahụ dị ka okpomoku ahịrị nnyefe. Okpomọkụ oven malitere site na 80 Celsius ma jide ya maka 5 min; ewelitere site na 15 Celsius C / min ruo 240 Celsius, wee rute 280 Celsius C na 25 Celsius C / min ma debe ya maka 5 min. Egosiri ọnọdụ MRM na Tebụl 3.

Nyocha ndekọ ọnụ ọgụgụ
A na-edozi ọdịnaya AQ dị n'ime akwụkwọ ọhụrụ ka ọ bụrụ ihe na-ekpo ọkụ site na ikesa ọdịnaya mmiri iji tụnyere ma nyochaa ọkwa AQ n'oge nhazi.

Ejiri sọftụ Microsoft Excel na IBM SPSS Statistics 20 tụlere mgbanwe AQ na nlele tii.

A na-eji ihe nhazi kọwapụta mgbanwe na AQ n'oge nhazi tii. PF = Rl / Rf , ebe Rf bụ ọkwa AQ tupu usoro nhazi na Rl bụ ọkwa AQ mgbe usoro nhazi gasịrị. PF na-egosi mbelata (PF <1) ma ọ bụ mmụba (PF> 1) na AQ fọdụrụnụ n'oge nhazi nhazi.

ME na-egosi mbelata (ME <1) ma ọ bụ mmụba (ME> 1) na nzaghachi na ngwa nyocha, nke dabere na oke mkpọda nke calibration na matrix na ihe mgbaze dị ka ndị a:

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

Ebe slopematrix bụ slope nke calibration curve na matrix-datched mgbaze, slopesolvent bụ mkpọda nke calibration curve na ihe mgbaze.

EKWESỊRỊ
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