1 ph\u1ea1m vi
\nTi\u00eau chu\u1ea9n n\u00e0y ch\u1ec9 \u0111\u1ecbnh ph\u01b0\u01a1ng ph\u00e1p ki\u1ec3m tra d\u01b0 l\u01b0\u1ee3ng chlorpyrifos trong th\u1ef1c ph\u1ea9m b\u1eb1ng ph\u00e9p s\u1eafc k\u00fd kh\u00ed -M\u00e1y d\u00f2 tr\u1eafc quang ng\u1ecdn l\u1eeda (GC -FPD) v\u00e0 ph\u00e9p s\u1eafc k\u00fd kh\u00ed -MASTROMYPRY (GC -MS).
\nTi\u00eau chu\u1ea9n n\u00e0y c\u00f3 th\u1ec3 \u00e1p d\u1ee5ng cho vi\u1ec7c x\u00e1c \u0111\u1ecbnh v\u00e0 x\u00e1c nh\u1eadn h\u00e0m l\u01b0\u1ee3ng d\u01b0 l\u01b0\u1ee3ng c\u1ee7a chlorpyrifos trong ng\u00f4, m\u00e0u n\u00e2u, h\u00e0nh l\u00e1, rau bina, \u1edbt, cam, t\u00e1o, h\u1ea1t th\u00f4ng -nut, tr\u00e0, m\u1eadt ong, c\u00e1, m\u1eadt ong, th\u1ecbt l\u1ee3n, th\u1eadn v\u00e0 gan g\u00e0.<\/p>\n
2 nguy\u00ean t\u1eafc<\/p>\n
M\u1eabu m\u00e0u cam ho\u1eb7c th\u1ef1c v\u1eadt kh\u00e1c \u0111\u01b0\u1ee3c chi\u1ebft b\u1eb1ng ethyl acetate.<\/p>\n
3 thu\u1ed1c th\u1eed v\u00e0 v\u1eadt li\u1ec7u<\/p>\n
T\u1ea5t c\u1ea3 c\u00e1c thu\u1ed1c th\u1eed \u0111\u01b0\u1ee3c s\u1eed d\u1ee5ng ph\u1ea3i \u0111\u01b0\u1ee3c ph\u00e2n t\u00edch tinh khi\u1ebft tr\u1eeb khi c\u00f3 quy \u0111\u1ecbnh kh\u00e1c.
\n3.1 Acetone: c\u1ea5p d\u01b0.<\/p>\n
3.2 Dichloromethane: c\u1ea5p d\u01b0.<\/p>\n
3.3 Cyclohexane: c\u1ea5p d\u01b0
\n3,4 ethyl acetate: c\u1ea5p d\u01b0.<\/p>\n
3,5 n-hexane: c\u1ea5p d\u01b0.<\/p>\n
3.6 Natium clorua dung d\u1ecbch n\u01b0\u1edbc.<\/p>\n
3.7 Natri Sulfate khan: \u0110\u1ed1t ch\u00e1y \u1edf 650 \u00b0 C trong 4H, sau \u0111\u00f3 \u0111\u01b0\u1ee3c l\u01b0u tr\u1eef trong th\u00f9ng ch\u1ee9a k\u00edn.
\n3.8 Dung d\u1ecbch n\u01b0\u1edbc natri clorua (5%): C\u00e2n natri clorua 5.0g.
\n3.9 Etyl axetat-n-Hexan (1+1V\/V) th\u1ec3 t\u00edch 100 mL Etyl axetat v\u00e0o b\u00ecnh Erlenmeyer 250 mL. sau \u0111\u00f3 th\u00eam 100 mL n-Hexan, tr\u1ed9n \u0111\u1ec1u.
\n3.9 Etyl axetat-n-Hexan (1+1V\/V) th\u1ec3 t\u00edch 100 mL Etyl axetat v\u00e0o b\u00ecnh Erlenmeyer 250 mL. sau \u0111\u00f3 th\u00eam 100 mL n-Hexan, tr\u1ed9n \u0111\u1ec1u.
\n3.11 Ti\u00eau chu\u1ea9n chlorpyrifos (C9 H11C13 NO3 PS, CAS s\u1ed1 2921-88-2) Tinh khi\u1ebft> 98%.<\/p>\n
3.12 Gi\u1ea3i ph\u00e1p ch\u1ee9ng kho\u00e1n ti\u00eau chu\u1ea9n: C\u00e2n b\u1eb1ng ch\u00ednh x\u00e1c m\u1ed9t s\u1ed1 l\u01b0\u1ee3ng nh\u1ea5t \u0111\u1ecbnh c\u1ee7a ti\u00eau chu\u1ea9n chlorpyrifos v\u00e0 dis - gi\u1ea3i quy\u1ebft n\u00f3 v\u1edbi m\u1ed9t kh\u1ed1i l\u01b0\u1ee3ng nh\u1ecf ethyl acetate.
\n3. 13 Gi\u1ea3i ph\u00e1p l\u00e0m vi\u1ec7c ti\u00eau chu\u1ea9n: Pha lo\u00e3ng dung d\u1ecbch g\u1ed1c ti\u00eau chu\u1ea9n v\u1edbi ethyl acetate v\u1edbi n\u1ed3ng \u0111\u1ed9 c\u1ea7n thi\u1ebft \u0111\u1ec3 t\u1ea1o ra gi\u1ea3i ph\u00e1p l\u00e0m vi\u1ec7c ti\u00eau chu\u1ea9n.
\n3.14 \u1ed1ng Florisil Spe: Florisil, 500 mg, 6ml ho\u1eb7c t\u01b0\u01a1ng \u0111\u01b0\u01a1ng.<\/p>\n
3. 15 \u1ed0ng carbon spe ho\u1ea1t \u0111\u1ed9ng: Envi -carb.250 mg, 6 ml ho\u1eb7c t\u01b0\u01a1ng \u0111\u01b0\u01a1ng.
\n3.16 B\u1ed9 l\u1ecdc m\u00e0ng: 0. 45 UM.<\/p>\n
3. 17 Graphitic Carbon: 60 L\u01b0\u1edbi ~ 80 L\u01b0\u1edbi<\/p>\n
4 b\u1ed9 m\u00e1y v\u00e0 thi\u1ebft b\u1ecb<\/p>\n
4. 1 GC: S\u1eafc k\u00fd kh\u00ed \u0111\u01b0\u1ee3c trang b\u1ecb FPD, 526nm.
\n4.2 GC -MS: \u0110\u01b0\u1ee3c trang b\u1ecb ngu\u1ed3n Electro -impact (EL).<\/p>\n
4. 3 M\u00e1y ly t\u00e2m: 4 000 v\u00f2ng\/ph\u00fat.<\/p>\n
4.4 GPC: \u0110\u01b0\u1ee3c trang b\u1ecb m\u00e1y b\u01a1m v\u00e0 b\u1ed9 thu ph\u00e2n s\u1ed1 isocrates.<\/p>\n
4. 5 Homogenizer.<\/p>\n
4. 6 M\u00e1y bay h\u01a1i ch\u00e2n kh\u00f4ng quay.<\/p>\n
4.<\/p>\n
4,8 Ph\u1ec5u t\u00e1ch: 250 ml<\/p>\n
4,9 Chai c\u00f4 \u0111\u1eb7c: 50 ml v\u00e0 250 ml<\/p>\n
4. 10 C\u00e2n b\u1eb1ng \u0111i\u1ec7n t\u1eed: ch\u00ednh x\u00e1c \u0111\u1ebfn 0. 000 1 g.<\/p>\n
4. 11 \u1ed1ng ly t\u00e2m nh\u1ef1a: 50 ml<\/p>\n
<\/p>\n
5 Chu\u1ea9n b\u1ecb v\u00e0 l\u01b0u tr\u1eef m\u1eabu th\u1eed nghi\u1ec7m
\n5.1 Chu\u1ea9n b\u1ecb m\u1eabu th\u1eed nghi\u1ec7m<\/p>\n
5.1.1 ng\u00f4, g\u1ea1o n\u00e2u, tr\u00e0, h\u1ea1t th\u00f4ng, \u0111\u1eadu ph\u1ed9ng v\u00e0 m\u1eadt ong<\/p>\n
L\u1ea5y kho\u1ea3ng 500 g m\u1eabu \u0111\u1ea1i di\u1ec7n.<\/p>\n
5.1.2 Cam, t\u00e1o, rau bina v\u00e0 h\u00e0nh l\u00e1<\/p>\n
L\u1ea5y kho\u1ea3ng 500 g m\u1eabu \u0111\u1ea1i di\u1ec7n.
\n5.1.3 Th\u1ecbt l\u1ee3n.<\/p>\n
M\u1ea5t kho\u1ea3ng 1 kg m\u1eabu \u0111\u1ea1i di\u1ec7n.
\n5.1.4 Chili<\/p>\n
L\u1ea5y kho\u1ea3ng 500 g m\u1eabu \u0111\u1ea1i di\u1ec7n.
\n5.2 L\u01b0u tr\u1eef m\u1eabu th\u1eed nghi\u1ec7m<\/p>\n
C\u00e1c m\u1eabu th\u1eed nghi\u1ec7m c\u1ee7a ng\u0169 c\u1ed1c, c\u00e1c lo\u1ea1i h\u1ea1t, tr\u00e0.
\n6 Th\u1ee7 t\u1ee5c<\/p>\n
6.1 Khai th\u00e1c<\/p>\n
6.1.1 Cam, t\u00e1o, rau bina, h\u00e0nh l\u00e1, ng\u00f4, m\u00e0u n\u00e2u, v\u00e0 \u1edbt<\/p>\n
C\u00e2n 10g (ch\u00ednh x\u00e1c \u0111\u1ebfn 0,01g) c\u1ee7a m\u1eabu th\u1eed nghi\u1ec7m v\u00e0o \u1ed1ng ly t\u00e2m 50 ml (4. 11).<\/p>\n
6.1.2 Tr\u00e0<\/p>\n
C\u00e2n 5g (ch\u00ednh x\u00e1c \u0111\u1ebfn 0,01 g) c\u1ee7a m\u1eabu th\u1eed nghi\u1ec7m v\u00e0o \u1ed1ng ly t\u00e2m nh\u1ef1a 50 ml.
\n6.1.3 Th\u1ecbt l\u1ee3n, gan g\u00e0, th\u1eadn g\u00e0, c\u00e1, h\u1ea1t th\u00f4ng -NET v\u00e0 \u0111\u1eadu ph\u1ed9ng<\/p>\n
C\u00e2n 20 g (ch\u00ednh x\u00e1c \u0111\u1ebfn 0,01g) (5g \u0111\u1ed1i v\u1edbi h\u1ea1t nh\u00e2n -net -net v\u00e0 \u0111\u1eadu ph\u1ed9ng) c\u1ee7a m\u1eabu th\u1eed nghi\u1ec7m v\u00e0o b\u00ecnh Erlenmeyer \u0111\u00f3ng b\u0103ng 250 ml.
\nChuy\u1ec3n chi\u1ebft xu\u1ea5t v\u00e0o m\u1ed9t ph\u1ec5u t\u00e1ch 250 ml.
\n6.2 L\u00e0m s\u1ea1ch -up<\/p>\n
6. 2. 1 GPC l\u00e0m s\u1ea1ch -up<\/p>\n
6.2.<\/p>\n
a) C\u1ed9t GPC: 700 mm x 25 mm (i. D.) Bio Beads S-X3 ho\u1eb7c t\u01b0\u01a1ng \u0111\u01b0\u01a1ng;<\/p>\n
B) Pha di \u0111\u1ed9ng: cyclohexane -ethyl acetate (1+1)<\/p>\n
C) T\u1ed1c \u0111\u1ed9 d\u00f2ng ch\u1ea3y: 4. 7 mL\/min:<\/p>\n
D) Kh\u1ed1i l\u01b0\u1ee3ng ti\u00eam t\u1ea1i v\u00f2ng m\u1eabu: 10ml:
\ne) Th\u1eddi gian b\u00e1n tr\u01b0\u1edbc: 10 ph\u00fat:<\/p>\n
f) Th\u1eddi gian c\u00e2n b\u1eb1ng GPC: 5 ph\u00fat:<\/p>\n
g) Th\u1eddi gian thu th\u1eadp c\u00e1c Eluates: 22 ph\u00fat ~ 31 ph\u00fat.
\nA) C\u1ed9t s\u1eafc k\u00fd: C\u1ed9t mao qu\u1ea3n Silica HP -5, 30 m x 0.<\/p>\n
b) Nhi\u1ec7t \u0111\u1ed9 c\u1ed9t: 50 \u00b0C (gi\u1eef 1 ph\u00fat) (30\u00b0C\/ph\u00fat) \u2013 180 \u00b0C (gi\u1eef 1 ph\u00fat) (10\u00b0 C\/ph\u00fat) \u2013 250\u00b0C (gi\u1eef 10 ph\u00fat).
\nC) Nhi\u1ec7t \u0111\u1ed9 c\u1ed5ng ti\u00eam: 250 C:<\/p>\n
d) Nhi\u1ec7t \u0111\u1ed9 giao di\u1ec7n: 250 C:<\/p>\n
e) Kh\u00ed mang: Nit\u01a1, \u0111\u1ed9 tinh khi\u1ebft > 99,999%, l\u01b0u l\u01b0\u1ee3ng 1,0 mL\/ph\u00fat:<\/p>\n
f) Th\u1ec3 t\u00edch ti\u00eam: 1 \u03bcl;<\/p>\n
g) Ch\u1ebf \u0111\u1ed9 ti\u00eam: Kh\u00f4ng chia t\u00e1ch.<\/p>\n
6.3.2 \u0110i\u1ec1u ki\u1ec7n ho\u1ea1t \u0111\u1ed9ng GC -MS<\/p>\n
A) C\u1ed9t s\u1eafc k\u00fd: C\u1ed9t mao qu\u1ea3n Silica HP -5.<\/p>\n
b) Nhi\u1ec7t \u0111\u1ed9 c\u1ed9t: 50 \u00b0C (gi\u1eef 2 ph\u00fat) (20\u00b0C\/ph\u00fat) \u2013 200 \u00b0C (gi\u1eef 1 ph\u00fat) (5\u00b0 C\/ph\u00fat) \u2013 270\u00b0C (gi\u1eef 18 ph\u00fat).
\nC) Nhi\u1ec7t \u0111\u1ed9 c\u1ed5ng ti\u00eam: 280 \u00b0 C<\/p>\n
d) Nhi\u1ec7t \u0111\u1ed9 giao di\u1ec7n: 280 \u00b0 C:<\/p>\n
E) Kh\u00ed mang: Helium.<\/p>\n
f) Th\u1ec3 t\u00edch ti\u00eam: 1 UL<\/p>\n
g) Ch\u1ebf \u0111\u1ed9 ti\u00eam: Kh\u00f4ng chia t\u00e1ch.<\/p>\n
h) Ch\u1ebf \u0111\u1ed9 ion h\u00f3a electron: EL:<\/p>\n
i) N\u0103ng l\u01b0\u1ee3ng ion h\u00f3a: 70 EV:<\/p>\n
j) Ch\u1ebf \u0111\u1ed9 x\u00e1c \u0111\u1ecbnh: SIM;<\/p>\n
k) C\u00e1c ion gi\u00e1m s\u00e1t \u0111\u01b0\u1ee3c ch\u1ecdn (m\/z); ion \u0111\u1ecbnh l\u01b0\u1ee3ng l\u00e0 197 v\u00e0 c\u00e1c ion x\u00e1c nh\u1eadn l\u00e0 258, 286, 314:
\nl) \u0110\u1ed9 tr\u1ec5 dung m\u00f4i 9. 0 ph\u00fat.
\n6.3.3 X\u00e1c \u0111\u1ecbnh GC<\/p>\n
Theo h\u00e0m l\u01b0\u1ee3ng g\u1ea7n \u0111\u00fang c\u1ee7a chlorpyrifos, ch\u1ecdn m\u1ed9t gi\u1ea3i ph\u00e1p l\u00e0m vi\u1ec7c ti\u00eau chu\u1ea9n c\u00f3 n\u1ed3ng \u0111\u1ed9 t\u01b0\u01a1ng t\u1ef1 c\u1ee7a dung d\u1ecbch m\u1eabu.