\u0130lke
\nPiridaben kal\u0131nt\u0131lar\u0131, GC-ECD ile belirlenen bir jel ge\u00e7irgenlik kromatografisi (GPC) veya SPE ile safla\u015ft\u0131r\u0131lan ve GC-MS taraf\u0131ndan onaylanan etil asetat-sikloheksan veya asetonitril ile ekstrakte edildi.<\/p>\n
Reaktifler ve Malzemeler
\nKullan\u0131lan t\u00fcm reaktifler aksi belirtilmedik\u00e7e analitik olarak saf olmal\u0131d\u0131r.
\n1. Etil Asetat: HPLC s\u0131n\u0131f\u0131.
\n2. Sikloheksan: HPLC s\u0131n\u0131f\u0131.
\n3. Asetonitril: HPLC s\u0131n\u0131f\u0131
\n4. Heksan: HPLC s\u0131n\u0131f\u0131.
\n5. Triklorometan: HPLC derecesi.
\n6. Susuz sodyum s\u00fclfat;
\n4 saat ve s\u0131k\u0131ca kapal\u0131 bir kapta tutuldu.
\n7. Sodyum klor\u00fcr.
\n8. Etil asetat + sikloheksan (1 + 1, V\/V).
\n9. Heksan + triklorometan (9 + 1, V\/V).
\n10. sikloheksan + etil asetat (6 + 1, V\/V)
\n11. Piridaben Standard\u0131 (Piridaben: CAS No. 96489-71-3: Molek\u00fcler Form\u00fcl C19H25cin2OS; Molek\u00fcler A\u011f\u0131rl\u0131k: 364. 93; Saf:).
\n12. Standart stok \u00e7\u00f6z\u00fcm\u00fc: Belli bir miktar piridaben standard\u0131n\u0131 do\u011fru bir \u015fekilde tart\u0131n ve k\u00fc\u00e7\u00fck bir hacim etil asetatta \u00e7\u00f6z\u00fcn.
\n13. Standart \u00e7al\u0131\u015fma \u00e7\u00f6zeltisi: Daha sonra standart stok \u00e7\u00f6zeltisini etil asetat ile standart \u00e7al\u0131\u015fma \u00e7\u00f6zeltisi olarak gerekli konsantrasyona seyreltin.
\n14. Karbon-PSA-T\u00fcp: 1ml, 50mg, 3ml asetonitril + etil asetat ile aktif (10)
\n15. HLB spe t\u00fcpleri: 3 mL, 60 mg veya e\u015fde\u011feri.
\n(9), ba\u015flamadan \u00f6nce 2 mL triklorometan ve 5 ml dam\u0131t\u0131lm\u0131\u015f su.
\n16. Film: 0.45 \u03bcm.<\/p>\n
Aparat ve ekipman
\n1. Gaz kromatografisi: ECD ile donat\u0131lm\u0131\u015f
\n2. Gaz kromatografisi: elektron iyonizasyon k\u00fctle spektrometrisi ile donat\u0131lm\u0131\u015ft\u0131r.
\n3. Analitik denge: 0.01 g duygusu.
\n4. Analitik denge: 0.1 mg duygusu
\n5. \u0130zokratik pompa ve fraksiyon koleksiyoncusu ile donat\u0131lm\u0131\u015f jel permeation kromatografi.
\n6. Santrif\u00fcj: 4000 d\/dk.
\n7. d\u00f6ner vakum buharla\u015ft\u0131r\u0131c\u0131s\u0131
\n8. Susuz sodyum s\u00fclfat kolonu: 7.5 cm x 1.5 cm (i. D.) 5 cm emici pamuk \u00fczerine yak\u0131tla doldurulmu\u015f susuz sodyum s\u00fclfat.
\n9. Vorteks mikseri.
\n10. Ultrasonik makine.
\n11. Homojener.
\n12. 50 ml Stoppered plastik santrif\u00fcj t\u00fcp\u00fc.<\/p>\n
Test \u00f6rne\u011finin haz\u0131rlanmas\u0131 ve depolanmas\u0131
\nTest \u00f6rne\u011finin haz\u0131rlanmas\u0131
\n1. Tah\u0131llar ve \u00c7ay
\n\u00d6rne\u011fin ca.
\n2. Meyve ve Sebzeler
\nBirle\u015fik birincil numune ca.<\/p>\n
3. Et ve et \u00fcr\u00fcnleri, f\u0131nd\u0131k
\nTemsilciyi yakla\u015f\u0131k 1 kg \u00f6rnek al\u0131n.<\/p>\n
Test \u00f6rneklerinin depolanmas\u0131
\nTah\u0131l, \u00e7ay, f\u0131nd\u0131k, sirke, bal ve bal \u00fcr\u00fcnlerinin test \u00f6rnekleri 0 \u2103 ~ 4 \u2103 aras\u0131nda saklanmal\u0131d\u0131r.<\/p>\n
Prosed\u00fcr
\n\u00c7\u0131karma
\n1. Sebzeler, meyveler.
\n50 mL'lik t\u0131pal\u0131 plastik santrif\u00fcj t\u00fcp\u00fcne 10 g (0,01 g hassasiyette) test numunesi tart\u0131l\u0131r, sonra 100oor\/dk'da 1 dakika homojenize edilerek ekstrakte edilen 20 mL etil asetat + siklohekzan eklenir, sonra 4000\/dk'da 3 dakika santrif\u00fcj edilir, s\u00fcpernatant\u0131 ba\u015fka bir temiz t\u00fcpe aktar\u0131l\u0131r ve ekstraksiyon prosed\u00fcr\u00fc tekrar 20 mL etil asetat + siklohekzan ile tekrarlan\u0131r. S\u00fcpernatanlar suyu uzakla\u015ft\u0131rmak i\u00e7in susuz sodyum s\u00fclfat kolonundan ge\u00e7irilir, efluant 150 mL'lik konsantre \u015fi\u015feye toplan\u0131r ve 40 \u2103'lik su banyosu olan d\u00f6ner buharla\u015ft\u0131r\u0131c\u0131 ile neredeyse kuruyana kadar yo\u011funla\u015ft\u0131r\u0131l\u0131r. Kal\u0131nt\u0131y\u0131 10,0 mL etil asetat siklohekzan ile \u00e7\u00f6z\u00fcn, 0,45 um'lik membran filtreden s\u00fcz\u00fcn ve ar\u0131nmay\u0131 bekleyin.<\/p>\n
2. Ceviz.
\nTest \u00f6rne\u011finin a\u011f\u0131rl\u0131\u011f\u0131 10 (0. 01 g'a kadar) 50 mL'l\u0131k bir durdurulmu\u015f plastik santrif\u00fcj t\u00fcp\u00fcne.<\/p>\n
3. \u00c7ay ve So\u011fan
\nA\u011f\u0131rl\u0131k 2. 5 g (0. 01 g'a do\u011fru), 50 mL'lik durdurulmu\u015f plastik santrif\u00fcj t\u00fcp\u00fcne, 15 mL dam\u0131t\u0131lm\u0131\u015f su ekleyin, 1 saat durun.
\nS\u00fcpernatanlar, suyu \u00e7\u0131karmak i\u00e7in susuz sodyum s\u00fclfat kolonundan ge\u00e7irilir, at\u0131k su 150 mL konsantre bir \u015fi\u015feye toplan\u0131r ve 40 \u2103 su banyosuna sahip bir d\u00f6ner buharla\u015ft\u0131r\u0131c\u0131 taraf\u0131ndan neredeyse kurumaya yo\u011funla\u015f\u0131r.<\/p>\n
Temizleme
\nSebze meyveleri, tah\u0131llar, ceviz, tavuk karaci\u011feri i\u00e7in GPC temizleme.
\n1. GPC \u00e7al\u0131\u015fma ko\u015fulu
\nA) GPC S\u00fctunu: 300 mm 10 mm (i. D.), biyo boncuklar S-X3 veya e\u015fde\u011feri:
\nb) Mobil faz: sikloheksan-etil asetat (1+1):
\nc) Ak\u0131\u015f h\u0131z\u0131: 4. 7 mL\/min:
\nd) \u00d6rnek d\u00f6ng\u00fcs\u00fcnde enjeksiyon hacmi: 5 ml:
\ne) El\u00fcat\u0131n toplanma zaman\u0131: 7.5 dk ~ 12.<\/p>\n
2. GPC temizleme ad\u0131m\u0131<\/p>\n
Daha \u00f6nce elde edilen \u00e7\u00f6z\u00fcm\u00fc ilk ad\u0131mda g\u00f6sterilen parametrelerle GPC s\u00fctununa aktar\u0131n.
\nEl\u00fcsyon temiz bir t\u00fcpe toplan\u0131r ve bir azot ak\u0131\u015f\u0131 alt\u0131nda 35 \u2103'de kuruluk i\u00e7in buharla\u015ft\u0131r\u0131l\u0131r ve belirleme ve konformasyon i\u00e7in 1.0 mL etil asetat i\u00e7inde yeniden \u00e7\u00f6z\u00fcl\u00fcr.<\/p>\n
3. Sirke ve bal i\u00e7in SPE temizleme
\nA\u011f\u0131rl\u0131k 2.5 g numuneler plastik bir santrif\u00fcj t\u00fcp\u00fcne, 5 mL dam\u0131t\u0131lm\u0131\u015f su ve 30 saniye i\u00e7in girdap ekleyin.<\/p>\n
4. \u00c7ay ve so\u011fan i\u00e7in SPE temizleme
\nDaha \u00f6nce elde edilen \u00e7\u00f6zeltiyi karbon pSA t\u00fcp\u00fcne aktar\u0131n, 1,5 mL sikloheksan + etil asetat ile durulay\u0131n.<\/p>\n
GC tespiti
\nGC \u00e7al\u0131\u015fma ko\u015fullar\u0131
\nA) S\u00fctun: DB-1301 30 m 0. 25 mm (i.d.) x 0. 25 um veya e\u015fde\u011feri;
\nB) Kolon S\u0131cakl\u0131\u011f\u0131: 50 \u2103 (20 \u2103\/dakika) - 200 \u2103 (5 \u2103\/dakika) - 260 \u2103 (10 dakika).
\nc) Enjeksiyon ba\u011flant\u0131 noktas\u0131 s\u0131cakl\u0131\u011f\u0131: 260 c:
\nD) ECD S\u0131cakl\u0131\u011f\u0131: 300 C:
\ne) Ta\u015f\u0131y\u0131c\u0131 Gaz: Azot (safl\u0131k>% 99.999 ak\u0131\u015f h\u0131z\u0131: 2 mL {{url_placeholder_0}});
\nf) Enjeksiyon modu: b\u00f6l\u00fcnmez.
\ng) Enjeksiyon hacmi: 1 ul.<\/p>\n
GC tespiti
\nNumune \u00e7\u00f6zeltisindeki piridaben kal\u0131nt\u0131lar\u0131n\u0131n yakla\u015f\u0131k konsantrasyonuna g\u00f6re, numune \u00e7\u00f6zeltisininkine benzer pik alan\u0131 olan standart \u00e7al\u0131\u015fma \u00e7\u00f6zeltisini se\u00e7in.
\nYukar\u0131daki GC ko\u015fullar\u0131 alt\u0131nda, piridabenin tutma s\u00fcresi yakla\u015f\u0131k 20. 9 dakikad\u0131r.<\/p>\n
GC-MS Onay\u0131
\nGC-MS \u00c7al\u0131\u015fma Ko\u015fullar\u0131
\nA) Kromatografik s\u00fctun: 30 m x 0. 25 mm (i. D.)
\n0. 25 um film kal\u0131nl\u0131\u011f\u0131 ve HP-5MS silika k\u0131lcal kolon veya e\u015fde\u011feri;
\nB) Kolon S\u0131cakl\u0131\u011f\u0131: 50 \u2103 (1 dakika tutun) (10 \u2103\/dk) - 280 \u2103 (10 dakika);
\nc) Enjeksiyon ba\u011flant\u0131 noktas\u0131 s\u0131cakl\u0131\u011f\u0131: 250 \u2103\uff1b
\nd) Aray\u00fcz s\u0131cakl\u0131\u011f\u0131: 280 \u2103;
\ne) elektron iyonizasyon modu: EL;
\nf) Lionizasyon Enerjisi: 70 eV:
\nG) Ta\u015f\u0131y\u0131c\u0131 Gaz: Helyum, Safl\u0131k> 99.9, ak\u0131\u015f h\u0131z\u0131 1.0 mL\/min:
\nh) Enjeksiyon modu: B\u00f6l\u00fcnmez, 0'dan sonra valfi a\u00e7\u0131n.
\n75 dk:
\ni) Enjeksiyon Hacmi: 1 UL:
\nJ) Tespit Modu: SIM:
\nK) Se\u00e7ilen izleme iyonlar\u0131 (m\/z):147, 309, 105:
\nl) Solvent koruma gecikmesi: 5.0 dakika.<\/p>\n
GC-MS Onay\u0131
\nYukar\u0131daki \u00e7al\u0131\u015fma ko\u015fuluna g\u00f6re, hem numune \u00e7\u00f6zeltisi hem de standart \u00e7al\u0131\u015fma \u00e7\u00f6zeltisi i\u00e7in ayn\u0131 tutma s\u00fcresinde bir tepe noktas\u0131 ortaya \u00e7\u0131km\u0131\u015fsa, standart \u00e7\u00f6zelti ve numune \u00e7\u00f6zeltisini analiz edin.<\/p>\n
Bo\u015f test
\nBo\u015f testi, numune eklenmeden yukar\u0131daki prosed\u00fcrlere g\u00f6re yap\u0131lacakt\u0131r.<\/p>\n
Kararl\u0131l\u0131k s\u0131n\u0131r\u0131
\n\u015eeftali, armut, ku\u015fkonmaz patates, m\u0131s\u0131r karabu\u011fday, bal, sirke, ceviz, rubit eti, tavuk eti, karides, \u00e7ay yapra\u011f\u0131, so\u011fan ve tavuk karaci\u011ferinin tayin limiti 0,01 mg\/kg'd\u0131r.<\/p>","protected":false},"excerpt":{"rendered":"
Principle The pyridaben residues were extracted with Ethyl acetate-Cyclohexane or Acetonitrile, purified by a gel permeation chromatography (GPC) or SPE, determinated by GC-ECD and confirmation by GC-MS. using external standard method. Reagents and materials All the reagents used should be analytically pure unless otherwise specified. “Water” is distilled water. 1. Ethyl acetate: HPLC grade. 2. […]<\/p>\n","protected":false},"author":1,"featured_media":3338,"comment_status":"open","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"_acf_changed":false,"footnotes":""},"categories":[73],"tags":[],"class_list":["post-2802","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-food-and-drugs"],"acf":[],"_links":{"self":[{"href":"https:\/\/www.pgeneral.com\/tr\/wp-json\/wp\/v2\/posts\/2802","targetHints":{"allow":["GET"]}}],"collection":[{"href":"https:\/\/www.pgeneral.com\/tr\/wp-json\/wp\/v2\/posts"}],"about":[{"href":"https:\/\/www.pgeneral.com\/tr\/wp-json\/wp\/v2\/types\/post"}],"author":[{"embeddable":true,"href":"https:\/\/www.pgeneral.com\/tr\/wp-json\/wp\/v2\/users\/1"}],"replies":[{"embeddable":true,"href":"https:\/\/www.pgeneral.com\/tr\/wp-json\/wp\/v2\/comments?post=2802"}],"version-history":[{"count":1,"href":"https:\/\/www.pgeneral.com\/tr\/wp-json\/wp\/v2\/posts\/2802\/revisions"}],"predecessor-version":[{"id":4305,"href":"https:\/\/www.pgeneral.com\/tr\/wp-json\/wp\/v2\/posts\/2802\/revisions\/4305"}],"wp:featuredmedia":[{"embeddable":true,"href":"https:\/\/www.pgeneral.com\/tr\/wp-json\/wp\/v2\/media\/3338"}],"wp:attachment":[{"href":"https:\/\/www.pgeneral.com\/tr\/wp-json\/wp\/v2\/media?parent=2802"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/www.pgeneral.com\/tr\/wp-json\/wp\/v2\/categories?post=2802"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/www.pgeneral.com\/tr\/wp-json\/wp\/v2\/tags?post=2802"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}