Nguy\u00ean t\u1eafc
\nC\u00e1c d\u01b0 l\u01b0\u1ee3ng pyridaben \u0111\u01b0\u1ee3c chi\u1ebft xu\u1ea5t b\u1eb1ng ethyl acetate-cyclohexane ho\u1eb7c acetonitril, \u0111\u01b0\u1ee3c tinh ch\u1ebf b\u1eb1ng s\u1eafc k\u00fd th\u1ea9m th\u1ea5u gel (GPC) ho\u1eb7c SPE, \u0111\u01b0\u1ee3c x\u00e1c \u0111\u1ecbnh b\u1edfi GC-ECD v\u00e0 x\u00e1c nh\u1eadn b\u1edfi GC-MS.<\/p>\n
Thu\u1ed1c th\u1eed v\u00e0 v\u1eadt li\u1ec7u
\nT\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.
\n1. Ethyl acetate: L\u1edbp HPLC.
\n2. Cyclohexane: L\u1edbp HPLC.
\n3. Acetonitrile: L\u1edbp HPLC
\n4. Hexane: L\u1edbp HPLC.
\n5. Trichloromethane: L\u1edbp HPLC.
\n6. Natri sunfat khan;
\n4 gi\u1edd v\u00e0 gi\u1eef trong m\u1ed9t th\u00f9ng ch\u1ee9a \u0111\u00f3ng ch\u1eb7t.
\n7. Natri clorua.
\n8. Ethyl acetate + cyclohexane (1 + 1,V\/V).
\n9. Hexane + trichloromethane (9 + 1,V\/V).
\n10. Cyclohexane + ethyl acetate (6 + 1,V\/V)
\n11. Ti\u00eau chu\u1ea9n Pyridaben (Pyridaben: CAS s\u1ed1 96489-71-3: C\u00f4ng th\u1ee9c ph\u00e2n t\u1eed C19H25CIN2OS; Tr\u1ecdng l\u01b0\u1ee3ng ph\u00e2n t\u1eed: 364. 93; tinh khi\u1ebft: 99%).
\n12. Gi\u1ea3i ph\u00e1p ch\u1ee9ng kho\u00e1n ti\u00eau chu\u1ea9n: C\u00e2n b\u1eb1ng ch\u00ednh x\u00e1c m\u1ed9t l\u01b0\u1ee3ng ti\u00eau chu\u1ea9n pyridaben nh\u1ea5t \u0111\u1ecbnh v\u00e0 gi\u1ea3i quy\u1ebft n\u00f3 trong m\u1ed9t kh\u1ed1i l\u01b0\u1ee3ng nh\u1ecf ethyl acetate.
\n13. Gi\u1ea3i ph\u00e1p l\u00e0m vi\u1ec7c ti\u00eau chu\u1ea9n: Sau \u0111\u00f3 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 nh\u01b0 l\u00e0 gi\u1ea3i ph\u00e1p l\u00e0m vi\u1ec7c ti\u00eau chu\u1ea9n.
\n14. Carbon-psa- \u1ed1ng: 1ml, 50mg, ho\u1ea1t \u0111\u1ed9ng v\u1edbi 3ml acetonitril + ethyl acetate (10)
\n15. C\u00e1c \u1ed1ng HLB SPE: 3 ml, 60 mg ho\u1eb7c t\u01b0\u01a1ng \u0111\u01b0\u01a1ng.
\n(9), 2 ml trichloromethane v\u00e0 5 ml n\u01b0\u1edbc c\u1ea5t tr\u01b0\u1edbc khi b\u1eaft \u0111\u1ea7u.
\n16 .. Phim: 0,45 m.<\/p>\n
Thi\u1ebft b\u1ecb v\u00e0 thi\u1ebft b\u1ecb
\n1. S\u1eafc k\u00fd kh\u00ed: \u0110\u01b0\u1ee3c trang b\u1ecb ECD
\n2. S\u1eafc k\u00fd kh\u00ed: \u0110\u01b0\u1ee3c trang b\u1ecb quang ph\u1ed5 kh\u1ed1i ion h\u00f3a electron.
\n3. C\u00e2n b\u1eb1ng ph\u00e2n t\u00edch: \u00dd ngh\u0129a 0,01 g.
\n4. C\u00e2n b\u1eb1ng ph\u00e2n t\u00edch: C\u1ea3m gi\u00e1c 0,1 mg
\n5. S\u1eafc k\u00fd th\u1ea9m th\u1ea5u gel \u0111\u01b0\u1ee3c trang b\u1ecb m\u00e1y b\u01a1m v\u00e0 b\u1ed9 thu ph\u00e2n s\u1ed1 isocrates.
\n6. Ly t\u00e2m: 4 000r\/min.
\n7. M\u00e1y bay h\u01a1i ch\u00e2n kh\u00f4ng quay
\n8. C\u1ed9t natri sunfat khan: 7,5 cm x 1,5 cm (i. D.) Nhi\u00ean li\u1ec7u \u0111\u1ea7y nhi\u00ean li\u1ec7u natri sunfat h\u00f3 n\u01b0\u1edbc tr\u00ean b\u00f4ng h\u1ea5p th\u1ee5 5 cm.
\n9. M\u00e1y tr\u1ed9n xo\u00e1y.
\n10. M\u00e1y si\u00eau \u00e2m.
\n11. Homogenizer.
\n12. 50 ml \u1ed1ng ly t\u00e2m nh\u1ef1a ch\u1eb7n.<\/p>\n
Chu\u1ea9n b\u1ecb v\u00e0 l\u01b0u tr\u1eef m\u1eabu th\u1eed nghi\u1ec7m
\nChu\u1ea9n b\u1ecb m\u1eabu th\u1eed nghi\u1ec7m
\n1. Ng\u0169 c\u1ed1c v\u00e0 tr\u00e0
\nQu\u00fd m\u1eabu cho ca.
\n2. Tr\u00e1i c\u00e2y v\u00e0 rau qu\u1ea3
\nM\u1eabu ch\u00ednh k\u1ebft h\u1ee3p \u0111\u01b0\u1ee3c gi\u1ea3m xu\u1ed1ng th\u00e0nh ca.<\/p>\n
3. Th\u1ecbt v\u00e0 c\u00e1c s\u1ea3n ph\u1ea9m th\u1ecbt, c\u00e1c lo\u1ea1i h\u1ea1t
\nL\u1ea5y \u0111\u1ea1i di\u1ec7n kho\u1ea3ng 1 kg m\u1eabu.<\/p>\n
L\u01b0u tr\u1eef c\u00e1c m\u1eabu th\u1eed nghi\u1ec7m
\nC\u00e1c m\u1eabu th\u1eed nghi\u1ec7m c\u1ee7a ng\u0169 c\u1ed1c, tr\u00e0, c\u00e1c lo\u1ea1i h\u1ea1t, gi\u1ea5m, m\u1eadt ong v\u00e0 m\u1eadt ong n\u00ean \u0111\u01b0\u1ee3c l\u01b0u tr\u1eef trong kho\u1ea3ng 0 \u2103 ~ 4.<\/p>\n
Th\u1ee7 t\u1ee5c
\nTr\u00edch xu\u1ea5t
\n1. Rau, tr\u00e1i c\u00e2y.
\nC\u00e2n 10 g (ch\u00ednh x\u00e1c \u0111\u1ebfn 0,01 g) m\u1eabu th\u1eed v\u00e0o \u1ed1ng ly t\u00e2m nh\u1ef1a c\u00f3 n\u00fat \u0111\u1eady 50 mL, sau \u0111\u00f3 th\u00eam 20 mL etyl axetat + xyclohexan \u0111\u00e3 chi\u1ebft xu\u1ea5t v\u1edbi \u0111\u1ed3ng nh\u1ea5t h\u00f3a \u1edf t\u1ed1c \u0111\u1ed9 100 oor\/ph\u00fat trong 1 ph\u00fat, sau \u0111\u00f3 ly t\u00e2m \u1edf t\u1ed1c \u0111\u1ed9 4000\/ph\u00fat trong 3 ph\u00fat, chuy\u1ec3n ph\u1ea7n d\u1ecbch n\u1ed5i sang \u1ed1ng s\u1ea1ch kh\u00e1c v\u00e0 l\u1eb7p l\u1ea1i quy tr\u00ecnh chi\u1ebft xu\u1ea5t v\u1edbi 20 mL etyl axetat + xyclohexan m\u1ed9t l\u1ea7n n\u1eefa. Ph\u1ea7n d\u1ecbch n\u1ed5i \u0111\u01b0\u1ee3c d\u1eabn qua c\u1ed9t natri sulfat khan \u0111\u1ec3 lo\u1ea1i b\u1ecf n\u01b0\u1edbc, thu th\u1eadp d\u1ecbch ch\u1ea3y ra v\u00e0o b\u00ecnh c\u00f4 \u0111\u1eb7c 150 mL v\u00e0 ng\u01b0ng t\u1ee5 \u0111\u1ebfn g\u1ea7n kh\u00f4 b\u1eb1ng m\u00e1y bay h\u01a1i quay v\u1edbi b\u1ed3n n\u01b0\u1edbc 40 \u2103. H\u00f2a tan ph\u1ea7n c\u1eb7n b\u1eb1ng 10,0 mL etyl axetat xyclohexan, l\u1ecdc qua b\u1ed9 l\u1ecdc m\u00e0ng 0,45 um v\u00e0 ch\u1edd tinh ch\u1ebf.<\/p>\n
2. Walnut.
\nTr\u1ecdng l\u01b0\u1ee3ng 10 (ch\u00ednh x\u00e1c \u0111\u1ebfn 0. 01 g) c\u1ee7a m\u1eabu th\u1eed v\u00e0o \u1ed1ng ly t\u00e2m nh\u1ef1a ch\u1eb7n 50 ml.<\/p>\n
3. Tr\u00e0 v\u00e0 h\u00e0nh t\u00e2y
\nTr\u1ecdng l\u01b0\u1ee3ng 2. 5 g (ch\u00ednh x\u00e1c \u0111\u1ebfn 0. 01 g) c\u00e1c m\u1eabu, v\u00e0o \u1ed1ng ly t\u00e2m nh\u1ef1a ch\u1eb7n 50 ml, th\u00eam 15 ml n\u01b0\u1edbc c\u1ea5t, \u0111\u1ee9ng trong 1h.
\nC\u00e1c ch\u1ea5t n\u1ed5i tr\u00ean b\u1ec1 m\u1eb7t \u0111\u01b0\u1ee3c truy\u1ec1n qua m\u1ed9t c\u1ed9t natri sunfat khan \u0111\u1ec3 lo\u1ea1i b\u1ecf n\u01b0\u1edbc, thu th\u1eadp n\u01b0\u1edbc th\u1ea3i v\u00e0o chai c\u00f4 \u0111\u1eb7c 150 ml v\u00e0 ng\u01b0ng t\u1ee5 g\u1ea7n nh\u01b0 kh\u00f4 b\u1edfi thi\u1ebft b\u1ecb bay h\u01a1i quay v\u1edbi b\u1ec3 n\u01b0\u1edbc 40.<\/p>\n
D\u1ecdn d\u1eb9p
\nGPC l\u00e0m s\u1ea1ch cho tr\u00e1i c\u00e2y rau qu\u1ea3, ng\u0169 c\u1ed1c, qu\u1ea3 \u00f3c ch\u00f3, gan g\u00e0.
\n1. \u0110i\u1ec1u ki\u1ec7n ho\u1ea1t \u0111\u1ed9ng GPC
\na) C\u1ed9t GPC: 300 mm 10 mm (i. D.), Bio Beads S-X3 ho\u1eb7c t\u01b0\u01a1ng \u0111\u01b0\u01a1ng:
\nB) Pha di \u0111\u1ed9ng: Cyclohexane-ethyl acetate (1+1):
\nC) T\u1ed1c \u0111\u1ed9 d\u00f2ng ch\u1ea3y: 4. 7 mL\/min:
\nD) Kh\u1ed1i l\u01b0\u1ee3ng ti\u00eam t\u1ea1i v\u00f2ng m\u1eabu: 5 ml:
\ne) Th\u1eddi gian thu th\u1eadp ch\u1ea5t r\u1eeda gi\u1ea3i: 7,5 ph\u00fat ~ 12.<\/p>\n
2. B\u01b0\u1edbc l\u00e0m s\u1ea1ch GPC<\/p>\n
Chuy\u1ec3n gi\u1ea3i ph\u00e1p thu \u0111\u01b0\u1ee3c tr\u01b0\u1edbc \u0111\u00f3 v\u00e0o c\u1ed9t GPC v\u1edbi c\u00e1c tham s\u1ed1 \u0111\u01b0\u1ee3c hi\u1ec3n th\u1ecb trong b\u01b0\u1edbc \u0111\u1ea7u ti\u00ean.
\nVi\u1ec7c r\u1eeda gi\u1ea3i \u0111\u01b0\u1ee3c thu th\u1eadp v\u00e0o m\u1ed9t \u1ed1ng s\u1ea1ch v\u00e0 bay h\u01a1i \u0111\u1ebfn kh\u00f4 \u1edf m\u1ee9c 35 \u2103 d\u01b0\u1edbi m\u1ed9t d\u00f2ng nit\u01a1 v\u00e0 \u0111\u01b0\u1ee3c ph\u00e2n ph\u1ed1i l\u1ea1i trong 1,0 ml ethyl acetate \u0111\u1ec3 x\u00e1c \u0111\u1ecbnh v\u00e0 c\u1ea5u tr\u00fac.<\/p>\n
3. SPE l\u00e0m s\u1ea1ch gi\u1ea5m v\u00e0 m\u1eadt ong
\nTr\u1ecdng l\u01b0\u1ee3ng 2,5 g m\u1eabu v\u00e0o \u1ed1ng ly t\u00e2m nh\u1ef1a, th\u00eam 5 ml n\u01b0\u1edbc c\u1ea5t v\u00e0 xo\u00e1y trong 30 gi\u00e2y.<\/p>\n
4. SPE l\u00e0m s\u1ea1ch tr\u00e0 v\u00e0 h\u00e0nh t\u00e2y
\nChuy\u1ec3n dung d\u1ecbch thu \u0111\u01b0\u1ee3c tr\u01b0\u1edbc \u0111\u00f3 v\u00e0o \u1ed1ng carbon-psa, r\u1eeda s\u1ea1ch v\u1edbi 1. 5 ml cyclohexane + ethyl acetate.<\/p>\n
X\u00e1c \u0111\u1ecbnh GC
\n\u0110i\u1ec1u ki\u1ec7n ho\u1ea1t \u0111\u1ed9ng c\u1ee7a GC
\na) C\u1ed9t: DB-1301 30 m 0. 25 mm (i.d.) x 0. 25 um ho\u1eb7c t\u01b0\u01a1ng \u0111\u01b0\u01a1ng;
\nb) Nhi\u1ec7t \u0111\u1ed9 c\u1ed9t: 50 (20 \u2103\/ph\u00fat) - 200 \u2103 (5 \u2103\/ph\u00fat) - 260 (10 ph\u00fat).
\nC) Nhi\u1ec7t \u0111\u1ed9 c\u1ed5ng ti\u00eam: 260 C:
\nD) Nhi\u1ec7t \u0111\u1ed9 ECD: 300 C:
\ne) kh\u00ed mang: nit\u01a1 (\u0111\u1ed9 tinh khi\u1ebft> 99,999% t\u1ed1c \u0111\u1ed9 d\u00f2ng ch\u1ea3y: 2 ml {{url_placeholder_0}});
\nF) Ch\u1ebf \u0111\u1ed9 ti\u00eam: Kh\u00f4ng chia t\u00e1ch.
\ng) Th\u1ec3 t\u00edch ti\u00eam: 1 ul.<\/p>\n
X\u00e1c \u0111\u1ecbnh GC
\nTheo n\u1ed3ng \u0111\u1ed9 g\u1ea7n \u0111\u00fang c\u1ee7a d\u01b0 l\u01b0\u1ee3ng pyridaben trong dung d\u1ecbch m\u1eabu, ch\u1ecdn gi\u1ea3i ph\u00e1p l\u00e0m vi\u1ec7c ti\u00eau chu\u1ea9n v\u1edbi di\u1ec7n t\u00edch c\u1ef1c \u0111\u1ea1i t\u01b0\u01a1ng t\u1ef1 nh\u01b0 dung d\u1ecbch m\u1eabu.
\nTrong c\u00e1c \u0111i\u1ec1u ki\u1ec7n GC tr\u00ean, th\u1eddi gian l\u01b0u c\u1ee7a Pyridaben l\u00e0 kho\u1ea3ng 20. 9 ph\u00fat.<\/p>\n
X\u00e1c nh\u1eadn GC-MS
\n\u0110i\u1ec1u ki\u1ec7n ho\u1ea1t \u0111\u1ed9ng c\u1ee7a GC-MS
\na) C\u1ed9t s\u1eafc k\u00fd: 30 m x 0. 25 mm (i. D.)
\n0. 25 \u0111\u1ed9 d\u00e0y m\u00e0ng um, v\u00e0 c\u1ed9t mao qu\u1ea3n silica HP-5MS ho\u1eb7c t\u01b0\u01a1ng \u0111\u01b0\u01a1ng;
\nb) Nhi\u1ec7t \u0111\u1ed9 c\u1ed9t: 50 (gi\u1eef 1 ph\u00fat) (10 \u2103\/ph\u00fat) - 280 (10 ph\u00fat);
\nC) Nhi\u1ec7t \u0111\u1ed9 c\u1ed5ng ti\u00eam: 250 \u2103\uff1b
\nd) Nhi\u1ec7t \u0111\u1ed9 giao di\u1ec7n: 280;
\nE) Ch\u1ebf \u0111\u1ed9 ion h\u00f3a electron: El;
\nF) N\u0103ng l\u01b0\u1ee3ng s\u01b0 t\u1eed: 70 EV:
\ng) kh\u00ed mang: helium, \u0111\u1ed9 tinh khi\u1ebft> 99. 999%, t\u1ed1c \u0111\u1ed9 d\u00f2ng ch\u1ea3y 1.0 mL\/min:
\nh) Ch\u1ebf \u0111\u1ed9 ti\u00eam: Kh\u00f4ng ph\u00e2n t\u00e1ch, m\u1edf van sau 0.
\n75 ph\u00fat:
\ni) Kh\u1ed1i l\u01b0\u1ee3ng ti\u00eam: 1 UL:
\nJ) Ch\u1ebf \u0111\u1ed9 x\u00e1c \u0111\u1ecbnh: SIM:
\nk) C\u00e1c ion gi\u00e1m s\u00e1t \u0111\u01b0\u1ee3c ch\u1ecdn (m\/z):: 147, 309, 105:
\nL) \u0110\u1ed9 tr\u1ec5 b\u1ea3o v\u1ec7 dung m\u00f4i: 5,0 ph\u00fat.<\/p>\n
X\u00e1c nh\u1eadn GC-MS
\nTheo \u0111i\u1ec1u ki\u1ec7n ho\u1ea1t \u0111\u1ed9ng \u1edf tr\u00ean, ph\u00e2n t\u00edch gi\u1ea3i ph\u00e1p ti\u00eau chu\u1ea9n v\u00e0 gi\u1ea3i ph\u00e1p m\u1eabu, n\u1ebfu c\u00f3 m\u1ed9t \u0111\u1ec9nh xu\u1ea5t hi\u1ec7n \u1edf c\u00f9ng th\u1eddi gian l\u01b0u cho c\u1ea3 hai gi\u1ea3i ph\u00e1p m\u1eabu v\u00e0 gi\u1ea3i ph\u00e1p l\u00e0m vi\u1ec7c ti\u00eau chu\u1ea9n.<\/p>\n
B\u00e0i ki\u1ec3m tra tr\u1ed1ng
\nB\u00e0i ki\u1ec3m tra tr\u1ed1ng s\u1ebd \u0111\u01b0\u1ee3c th\u1ef1c hi\u1ec7n theo c\u00e1c quy tr\u00ecnh tr\u00ean m\u00e0 kh\u00f4ng c\u1ea7n th\u00eam m\u1eabu.<\/p>\n
Gi\u1edbi h\u1ea1n x\u00e1c \u0111\u1ecbnh
\nGi\u1edbi h\u1ea1n x\u00e1c \u0111\u1ecbnh c\u1ee7a \u0111\u00e0o, l\u00ea, m\u0103ng t\u00e2y, khoai t\u00e2y, ng\u00f4, ki\u1ec1u m\u1ea1ch, m\u1eadt ong, gi\u1ea5m, \u00f3c ch\u00f3, th\u1ecbt rubit, th\u1ecbt g\u00e0, t\u00f4m, l\u00e1 tr\u00e0, h\u00e0nh t\u00e2y v\u00e0 gan g\u00e0 l\u00e0 0,01 mg\/kg.<\/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\/vi\/wp-json\/wp\/v2\/posts\/2802","targetHints":{"allow":["GET"]}}],"collection":[{"href":"https:\/\/www.pgeneral.com\/vi\/wp-json\/wp\/v2\/posts"}],"about":[{"href":"https:\/\/www.pgeneral.com\/vi\/wp-json\/wp\/v2\/types\/post"}],"author":[{"embeddable":true,"href":"https:\/\/www.pgeneral.com\/vi\/wp-json\/wp\/v2\/users\/1"}],"replies":[{"embeddable":true,"href":"https:\/\/www.pgeneral.com\/vi\/wp-json\/wp\/v2\/comments?post=2802"}],"version-history":[{"count":1,"href":"https:\/\/www.pgeneral.com\/vi\/wp-json\/wp\/v2\/posts\/2802\/revisions"}],"predecessor-version":[{"id":4305,"href":"https:\/\/www.pgeneral.com\/vi\/wp-json\/wp\/v2\/posts\/2802\/revisions\/4305"}],"wp:featuredmedia":[{"embeddable":true,"href":"https:\/\/www.pgeneral.com\/vi\/wp-json\/wp\/v2\/media\/3338"}],"wp:attachment":[{"href":"https:\/\/www.pgeneral.com\/vi\/wp-json\/wp\/v2\/media?parent=2802"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/www.pgeneral.com\/vi\/wp-json\/wp\/v2\/categories?post=2802"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/www.pgeneral.com\/vi\/wp-json\/wp\/v2\/tags?post=2802"}],"curies":[{"name":"WP","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}