1 Kapsam
\nBu standart, g\u0131dalardaki klorpirifos tortusunu gaz kromatografisi -alev fotometrik dedekt\u00f6r (GC -FPD) ve gaz kromatografisi -k\u00fctlesi spektrometrisi (GC -MS) ile test etme y\u00f6ntemini belirtir.
\nBu standart, m\u0131s\u0131r, kahverengi, ye\u015fil so\u011fan, \u0131spanak, biber, portakal, elma, \u00e7am -nut \u00e7ekirde\u011fi, \u00e7ay, bal\u0131k, bal, domuz, tavuk b\u00f6brek ve tavuk karaci\u011finde klorpirifos kal\u0131nt\u0131s\u0131 i\u00e7eri\u011finin belirlenmesi ve do\u011frulanmas\u0131 i\u00e7in ge\u00e7erlidir.<\/p>\n
2 \u0130lke<\/p>\n
Turuncu veya di\u011fer bitkisel numune etil asetat ile ekstrakte edilir.<\/p>\n
3 reaktif ve malzeme<\/p>\n
Kullan\u0131lan t\u00fcm reaktifler aksi belirtilmedik\u00e7e analitik olarak saf olmal\u0131d\u0131r.
\n3.1 Aseton: Kal\u0131nt\u0131 derecesi.<\/p>\n
3.2 Diklorometan: Kal\u0131nt\u0131 derecesi.<\/p>\n
3.3 sikloheksan: kal\u0131nt\u0131 derecesi
\n3.4 Etil Asetat: Kal\u0131nt\u0131 S\u0131n\u0131f\u0131.<\/p>\n
3.5 n-heksan: kal\u0131nt\u0131 derecesi.<\/p>\n
3.6 Sodyum Klor\u00fcr Sulu \u00c7\u00f6zelti.<\/p>\n
3.7 Susuz sodyum s\u00fclfat: 4 saat boyunca 650 \u00b0 C'de tutu\u015fur ve daha sonra s\u0131k\u0131ca kapal\u0131 kapta saklan\u0131r.
\n3.8 Sodyum Klor\u00fcr Sulu \u00c7\u00f6zelti (%5): Sodyum klor\u00fcr 5.0g.
\n3.9 Etil asetat-n-Hekzan (1+1V\/V) hacmi 100 mL Etil asetat 250 mL Erlenmeyer \u015fi\u015fesine konulur. Daha sonra 100 mL n-Hekzan eklenir, kar\u0131\u015ft\u0131r\u0131l\u0131r.
\n3.9 Etil asetat-n-Hekzan (1+1V\/V) hacmi 100 mL Etil asetat 250 mL Erlenmeyer \u015fi\u015fesine konulur. Daha sonra 100 mL n-Hekzan eklenir, kar\u0131\u015ft\u0131r\u0131l\u0131r.
\n3.11 Klorpirifos Standard\u0131 (C9 H11C13 NO3 PS, CAS No. 2921-88-2) Safl\u0131k>.<\/p>\n
3.12 Standart Stok \u00c7\u00f6z\u00fcm\u00fc: Belirli miktarda klorpirifos standard\u0131 ve dis - k\u00fc\u00e7\u00fck bir hacim etil asetat ile \u00e7\u00f6z\u00fcn.
\n3. 13 Standart \u00c7al\u0131\u015fma \u00c7\u00f6z\u00fcm\u00fc: Standart \u00e7al\u0131\u015fma \u00e7\u00f6zeltisini yapmak i\u00e7in standart stok \u00e7\u00f6zeltisini etil asetat ile gerekli konsantrasyona seyreltin.
\n3.14 Florisil Spe T\u00fcp: Florisil, 500 mg, 6ml veya e\u015fde\u011feri.<\/p>\n
3. 15 Aktif karbon spe t\u00fcp\u00fc: Envi -carb.250 mg, 6 ml veya e\u015fde\u011feri.
\n3.16 Membran Filtresi: 0. 45 um.<\/p>\n
3. 17 Grafitik Karbon: 60 Mesh ~ 80 Mesh<\/p>\n
4 aparat ve ekipman<\/p>\n
4. 1 GC: FPD ile donat\u0131lm\u0131\u015f gaz kromatografisi, 526 nm.
\n4.2 GC -MS: Electro -Etki Kayna\u011f\u0131 (EL) ile donat\u0131lm\u0131\u015ft\u0131r.<\/p>\n
4. 3 Santrif\u00fcj: 4 000 d\/dk.<\/p>\n
4.4 GPC: \u0130zokratik pompa ve fraksiyon toplay\u0131c\u0131 ile donat\u0131lm\u0131\u015ft\u0131r.<\/p>\n
4. 5 homojenle\u015ftirici.<\/p>\n
4. 6 d\u00f6ner vakum buharla\u015ft\u0131r\u0131c\u0131.<\/p>\n
4. 7 Durdurulmu\u015f Erlenmeyer \u015ei\u015fesi: 250 ml<\/p>\n
4.8 Ayr\u0131l\u0131k Huni: 250 ml<\/p>\n
4.9 Konsantre \u015ei\u015fe: 50 ml ve 250 ml<\/p>\n
4. 10 Elektronik Denge: 0.000 1 g.<\/p>\n
4. 11 Plastik Santrif\u00fcj T\u00fcp\u00fc: 50 ml<\/p>\n
<\/p>\n
5 Test \u00f6rne\u011finin haz\u0131rlanmas\u0131 ve depolanmas\u0131
\n5.1 Test \u00f6rne\u011finin haz\u0131rlanmas\u0131<\/p>\n
5.1.1 M\u0131s\u0131r, kahverengi pirin\u00e7, \u00e7ay, \u00e7am f\u0131st\u0131\u011f\u0131 \u00e7ekirde\u011fi, f\u0131st\u0131k ve bal<\/p>\n
Yakla\u015f\u0131k 500 g temsili \u00f6rnek al\u0131n.<\/p>\n
5.1.2 Portakal, Elma, Ispanak ve Ye\u015fil Ye\u015fill\u00fck<\/p>\n
Yakla\u015f\u0131k 500 g temsili \u00f6rnek al\u0131n.
\n5.1.3 Domuz eti.<\/p>\n
Yakla\u015f\u0131k 1 kg temsili \u00f6rnek al\u0131n.
\n5.1.4 Chili<\/p>\n
Yakla\u015f\u0131k 500 g temsili \u00f6rnek al\u0131n.
\n5.2 Test \u00f6rne\u011finin depolanmas\u0131<\/p>\n
Tah\u0131l, f\u0131nd\u0131k, \u00e7ay test \u00f6rnekleri.
\n6 Prosed\u00fcr<\/p>\n
6.1 \u00c7\u0131karma<\/p>\n
6.1.1 Portakal, elma, \u0131spanak, ye\u015fil so\u011fan, m\u0131s\u0131r, kahverengi ve biber<\/p>\n
Test \u00f6rne\u011finin 10g (0.01g'ye do\u011fru) 50 mL'lik bir santrif\u00fcj t\u00fcp\u00fcne tart\u0131n (4. 11).<\/p>\n
6.1.2 \u00c7ay<\/p>\n
Test numunesinin 5g'yi (0.01 g'a kadar do\u011fru) 50 mL'lik bir plastik santrif\u00fcj t\u00fcp\u00fcne tart\u0131n.
\n6.1.3 Domuz eti, tavuk karaci\u011feri, tavuk b\u00f6bre\u011fi, bal\u0131k, \u00e7am -a\u011f \u00e7ekirde\u011fi ve f\u0131st\u0131k<\/p>\n
250 mL'lik durdurulmu\u015f Erlenmeyer \u015fi\u015fesine 20 g (\u00c7am a\u011f \u00e7ekirde\u011fi ve f\u0131st\u0131k i\u00e7in 5g (5g \u00c7am -a\u011f \u00e7ekirde\u011fi i\u00e7in 5g).
\nEkstrakt\u0131 bir 250 mL ay\u0131r\u0131c\u0131 huniye aktar\u0131n.
\n6.2 Temizlik -up<\/p>\n
6. 2. 1 GPC Temizleme -up<\/p>\n
6.2.<\/p>\n
A) GPC s\u00fctunu: 700 mm x 25 mm (i. D.) Biyo boncuklar S-X3 veya e\u015fde\u011feri;<\/p>\n
b) Mobil faz: sikloheksan -etil asetat (1+1)<\/p>\n
c) Ak\u0131\u015f h\u0131z\u0131: 4. 7 mL\/min:<\/p>\n
d) \u00d6rnek d\u00f6ng\u00fcs\u00fcnde enjeksiyon hacmi: 10ml:
\ne) \u00d6n kesme s\u00fcresi: 10 dakika:<\/p>\n
f) GPC Denge S\u00fcresi: 5 dakika:<\/p>\n
g) Eluatlar\u0131n toplanma zaman\u0131: 22 dk ~ 31 dk.
\nA) Kromatografik Kolon: HP -5 Silika K\u0131lcal S\u00fctun, 30 M x 0. 25 mm (i. D.) Film Kal\u0131nl\u0131\u011f\u0131 0. 25 U m veya e\u015fde\u011feri:<\/p>\n
b) Kolon s\u0131cakl\u0131\u011f\u0131: 50 \u00b0C (1 dk. tutun) (30 \u00b0C\/dk.) \u2013 180 \u00b0C (1 dk. tutun) (10 \u00b0C\/dk.) \u2013 250 \u00b0C (10 dk. tutun).
\nc) Enjeksiyon ba\u011flant\u0131 noktas\u0131 s\u0131cakl\u0131\u011f\u0131: 250 c:<\/p>\n
D) Aray\u00fcz S\u0131cakl\u0131\u011f\u0131: 250 C:<\/p>\n
e) Ta\u015f\u0131y\u0131c\u0131 gaz: Azot, safl\u0131k > ,999, ak\u0131\u015f h\u0131z\u0131 1,0 mL\/dak:<\/p>\n
f) enjeksiyon hacmi: 1 uL;<\/p>\n
g) Enjeksiyon modu: b\u00f6l\u00fcnmez.<\/p>\n
6.3.2 GC -Ms \u00c7al\u0131\u015fma Ko\u015fullar\u0131<\/p>\n
A) Kromatografik kolon: HP -5 Silika K\u0131lcal Kolon.<\/p>\n
b) Kolon s\u0131cakl\u0131\u011f\u0131: 50 \u00b0C (2 dk tutun) (20\u00b0C\/dk) \u2013 200 \u00b0C (1 dk tutun) (5\u00b0 C\/dk) \u2013 270\u00b0C (18 dk tutun).
\nc) Enjeksiyon ba\u011flant\u0131 noktas\u0131 s\u0131cakl\u0131\u011f\u0131: 280 \u00b0 C<\/p>\n
d) Aray\u00fcz s\u0131cakl\u0131\u011f\u0131: 280 \u00b0 C:<\/p>\n
e) Ta\u015f\u0131y\u0131c\u0131 Gaz: Helyum.<\/p>\n
f) enjeksiyon hacmi: 1 ul<\/p>\n
g) Enjeksiyon modu: b\u00f6l\u00fcnmez.<\/p>\n
H) Elektron \u0130yonizasyon Modu: EL:<\/p>\n
i) \u0130yonizasyon Enerjisi: 70 eV:<\/p>\n
J) Tespit Modu: SIM;<\/p>\n
k) Se\u00e7ilmi\u015f izleme iyonlar\u0131 (m\/z); kantifikasyon iyonu 197 ve do\u011frulama iyonlar\u0131 258, 286, 314't\u00fcr:
\nl) \u00c7\u00f6z\u00fcc\u00fc gecikmesi 9. 0 dakika.
\n6.3.3 GC Tespiti<\/p>\n
Klorpirifos'un yakla\u015f\u0131k i\u00e7eri\u011fine g\u00f6re, \u00f6rnek \u00e7\u00f6zeltisinin benzer konsantrasyonuna sahip bir standart \u00e7al\u0131\u015fma \u00e7\u00f6z\u00fcm\u00fc se\u00e7in.