KHOA
-
QUY IMIDACLOPRID AZOXYSTROBIN U CAO
Sinh Th.s. MSSV: 12D720401175 7B
2017
KHOA
Qua 5
-
khoa cho em
em
t
trong gia em xin
em
n
,
Ths. Ng
em trong em trong em
khai dung
trong ra
QUY IMIDACLOPRID AZOXYSTROBIN CAO
em ,
em
em
xin nh ng
em
cho C
, Sinh
Sinh Th.s. MSSV: 12D720401175 7B
2017
6
2017
Hai u
imidacloprid tin d
hai ,
azoxystrobin
cao trong
imidacloprid
azoxystrobin
trong .......................................................................................................................i
ra hai
N azoxystrobin
cao (HPLC). RP- C18 (250 x 4,6mm, 45%), trong azoxystrobin l
trong pha
gian 15 0,0048 ppm
acetonitril 250 nm. Gi quan
0,997.
RSD < 2%. V imidacloprid azoxystrobin
n
1.1.
......................................................................................................1
c (55%:
1.2.
...........................................................................................................1 ......................................................................2
hai
pic
imidacloprid trong
0,9978 98-102%
quy
: imidacloprid, azoxystrobin,
u
a imidacloprid
0,048 ppm.
quan azoxystrobin
.................................................................................................1
quy
imidacloprid
hai
ng, HPLC.
nhanh trong
2.1.
.................................................2
2.1.1.
...............................................................2
2.1.2.
.................................................................2
2.1.3. Imidacloprid ...................................................................................................3 ................................................................................................3 2.1.3.
.....................................................................................................3 .....................................................................3
2.1.3.4
.......................................................................4 ...........................................................4
2.1.4. Azoxystrobin ..................................................................................................5 ................................................................................................5 .....................................................................................................5 .....................................................................5 .......................................................................5 .......................................................................................6 ..........6 ....................................................6 .... 6 ...8 2.1.6.3. Ph azoxystrobin. ........................................................................................................8 i
.......9
........................................................................19
.......................................................................................................9
...........................................................................20
.........................................................................................................9
.......................................................21
........................................................9
..............................................................................21
..............................................................................10
.......................................................................................................21
....................................................................................10
.............................................................................................21
............................................................................................11
...............................................................................................21
..................................................................................11
........................................................................................21
..............................................................................................11
....................................................................................................21
...................................................................................................11
.................................................................................................22
..............................................................................11
...............................................................................22
..................................................................................12
......................................................................23
....................................................12 2.2.5.
-
3.3.1. Chu
......................................................................................23
......................................................................12
.............................................23
............................................................13
.................................................................................................23
....................................................................................13
................................................................23
....................................................................................14
.................................................23
.............................................................................14
..............................................................24
...........................................................................................15
.............................................................................25
......................................................................................15
..............................................................................25
....................................................................................15
...........................................................................25
...................................16
.........................................................................................26
.............................................................16
...........27
..................................................................................17
......................................................................................27
................................................................................17
..........................................................................................28
............................................................................19
...................................................................28
..............................................................19
.......................................................29
................................................................19
..................................................................30
ii
iii
...30
DANH
......................................................................................30 4.1.2 K
..............................................................30 ...................................................................30
ACN
:
As
: :
..............................................................31 ..............................................................................35
Acetonitrile
HPLC
:
Nam High Performance Liquid Chromatography cao)
...............................................................35
LC50
:
Lethal concentration (
.....................................................................................35
LD50
:
Lethal dose
..........................................................................35
LOD
:
Limit of quantitation
LOQ
:
Limit of detection
PDA
:
Photo Diode Array
..........................................................................................38 ......................................................39 ......................................................................................40
50% ) 50%)
diod quang)
ppm
:
Part per million (p
Rs
:
Resolution
RSD
:
Relative Standard Deviation
SD
:
Standard Deviation
..........................................................................................43 .................................................................................................45 .....................................................................................................47 .................................................................48
Speak
:
.........................................................................................................48
UV
:
...........................................................................................................49
Vis
:
pic
...........................................................................................50
iv
v
DANH
DANH
2.1.
...............................................................................3
2.2.
zoxystrobin ...............................................................................5
3.
.........................................................................9
2.1.
....................................................4 ...................................................6
3
................................................................18 m
................................................14 D
................31
..............................21 -
......................21
..............................................................32
......................................24
5%:5%). ................................................................32
............................36
...............................................................33
..................................37
..............................................................33 ...............................................................................40
..............................................................34
...........41
..............................................................34
...........41
.........................................36
..............................43
................38
..................................43
....................39 ..................39
8.
..............................44 ......................................44
...42
....................................45
..42
...........45 ...................46
azoxystrobin...................................................................................................................48
vi
vii
1.
2.
1.1. Trong
2.1. 2.1.1.
nguy n m...
t
vai
QUAN
QUAN
h
quan nay, khi
hay cho
bao ng
gian
con
trung mong
d trong azoxystrobin
imidacloprid
mua
ng hai
hay
trong trong
c trong
imidacloprid
VIS,
sinh
azoxystrobin : quang UVcho
cao (HPLC)
HPLC cao
nay
sau khi thu
trong
do cho
,
so
Cao
2.1.2. theo ba
khoa
-
t
:
.
an ch
.
trong hai hai
ng
nhanh,
nguy
thay
imidacloprid
.
sinh
con
trong
(Saed Mousa Diab Ali, 2012).
trong
cao (HPLC). imidacloprid
bao
imidacloprid, dichlopropene, methyl isocyanate, chloropicrin, methyl bromide aldicarb, dazomet metham natri, qua
trong
nhanh
Trong
sau:
t
cao (HPLC)
azoxystrobin
2015).
-
quy
Hormon trong
azoxystrobin mong ra
tan g
ph
1.2. M
trong t
2,4,5-T; 2,4-D;
cao
bao
trong dintrophenols, xianophenols, pentachlorophenol
Paraquat (Saed Mousa Diab Ali, 2012). hai imidacloprid HPLC
- Th
sau: azoxystrobin
detector UV-VIS. quy
h
l
imidacloprid
hay
vi
nhau nhau.
azoxystrobin.
carbamat
benomyl. vi sinh
trong t 1
gian
(Saed Mousa Diab Ali, 2012). 2
t trong
hai
Trong imidacloprid
-
azoxystrobin. Theo
trong
pH
5-11, khi
nh
n
cao, sinh ra
Imidacloprid (Raihanah, 2016)
2.1.3.4.
azoxystrobin
imidacloprid D
0.
m. Theo
ra
, imidacloprid trong
. 2.1:
2.1.3. Imidacloprid 2.1.3.1. Imidacloprid
tin
t
imidacloprid
trong
LD50
trong Pyridin
Clo
cao
sau:
ng Azo 5
LD50 > 5000 mg/kg
da
(Sacramento, 2002).
130 mg/kg
da
[31]
2.1.3.2.
LC50 > 5,33 mg/l
t, run
2.1. chung
-
imidacloprid
imidacloprid
-
Trong
C9H10ClN5O2
-
255,662 g/mol
- Danh IUPAC: N-[1-[(6-chloropyridin-3-yl)methyl]-4,5dihydroimidazol-2-yl]nitramide -
HCBVTV:
-
(Spivastava, 2004).
imidacloprid
Neonicotinoid
tinh
-
1.54 g/cm3
cho 0,06 mg/kg
Imidacloprid
be,
Imidacloprid
o
1.00 x 10-7 mm Hg (20 C) trong tan trong gian
Neonicotinoid nicotin. acetylcholin,
receptor
144 C
-
n
kinh o
-
(ADI) trong (Spivastava, 2004). imidacloprid (Spivastava, 2004)
2.1.3.5.
(Sprivastava, 2004)
-
-
imidacloprid trong
t
2.1.3.3.
-
Imidacloprid bao
cao
g
kinh
qua da ng
0,61 g/l (20oC) o
30
(25 C
tan: Tan trong isopropanol, toluene 20oC
dung 3
do kinh trung
cho
pH 7) dchloromethane,
qua
nhanh trong trong
48 4
.
2.2.
2.1.4. Azoxystrobin (Bursic Vojislava and Lazic Sanja, 2012)
tin
azoxystrobin
2.1.4.1. Azoxystrobin b nh
m t lo i thu c di t n m ph r ng
nhi u
qu
ho t
ch ng l i m t s LD50 > 2000 mg / kg.
c nh nh m
Kh 2.1.4.2.
LD50 > 2000 mg / kg da
LC50
0,38 mg /l trong
da 2.2. -
chung
da
: Azoxystrobin
-
C22H17N3O5 403,4 g/mol
- Danh
da
azoxystrobin
L
cho
azoxystrobin
IUPAC: Methyl (E)-2-[2-[6-(2-cyanophenoxy)pyrimidin-4-
m
(ADI) trong
0-0,2 mg/ kg
(T.Nageswara Rao
(T.Nageswara Rao
2.1.4.5.
2012).
2012).
yl]oxyphenyl]-3-methoxyprop-2-enoate. -
HCBVTV:
-
Azoxystrobin
m
methocyacrylate. strobilurin
methoxyacrylates ty
trong
(Rao Nageswara, 2012)
2.1.4.3. -
tinh
-
1.25 g/cm3 ( 25 trong
-
ra.
tan: Tan trong
- Danh
imidacloprid
azoxystrobin
imidacloprid: Confidor 100 SL, Actador 100WP,
Javidan 100 WP, Anvado 100WP, Conphai 10WP, Kola 700WO, Abamix 1,45SP, dung
hexane, methanol, toluen, acetone, 20oC.
ethyl acetat, acetonitril, dichloromethane, -
th
2.1.5.
116 oC
khi
cao, sinh ra
Aba- plus 100EC
[32]
- Danh
nitrogen oxide (N2O)
azoxystrobin: Amistar Top 250 SC, Amistar Top
325 SC, Mi stop 350 SC, Ohho 3255SC, Neoamistagold 360SC, 400SC, 450SC, 500SC, Ammisdotop 400SC, Dovatop 400SC , Paramax 400SC[34].
2.1.4.4.
a azoxystrobin (Sh.A.Ashorkr, 2006) C
Theo
T.Nageswara Rao
2012
azoxystrobin qua
trong .
sau: 2.1.6. T
trong
2.1.6.1.
ng imidacloprid 1(J.Serb, 2009)
5
6
HPLC
C18 (250 cm x 4,6 mm, 5
-
azoxysrobin
2.1.6.2.
UV-Vis
1 (Bursic Vojilava and Lazic Sanja, 2012):
: acetonitril / 0,01 M dung
- Pha 25%: 75%
phosphate (pH 3.0) -
-
UV-Vis
- Pha -
25oC
-
C18 (250 cm x 4,6 mm, 5
-
1
-
270 nm 20
: acetonitril 80% : n 1
2 (Sacramento, 2002): -
20
-
gian
C18 (25 cm x 4,6 mm, 5
azoxystrobin: 11,07
.
2 (Burket and Sapiests, 2005):
UV-Vis
- Pha -
: acetonitril 30% : 1
-
-
70%
gian
UV-Vis : acetonitril 55% : n
-T -
20
-
RP C18 (25 cm x 4,6 mm, 5
- Pha
270 nm
-
imidacloprid: 5,5
-
20
-
gian
C18 (75 cm x 4,6 mm, 3,5 QuEChERS
- Pha
: acetonitril 20%:
-
C18 (250 cm x 4,6 mm, 5
-
80%
-
t
UV-Vis
- Pha -
: 270 nm
-
20
: acetonitril 70% : acid formic 30% 1
4 (Raihanah, 2004): - Pha
: acetonitril 20% : n
240 nm
-
C18 (25 cm x 4,6 mm, 5 UV-Vis
-
azoxystrobin: 8,3 3 (Rao Nageswara, 2012):
1
-
20 hai
2.1.6.3. Ph 80% trong imidacloprid ng
270 nm
-
t imidacloprid
azoxystrobin.
1
-
45%
1 207 nm
3 (Sprivastava, 2004):
10 (LOQ),
hai
azoxystrobin hai ng
p (LOD), gian),
20%
255 nm
-
-
HPLC
HPLC. N HPLC.
imidacloprid
azoxystrobin hay
trung cho
quan cao,
trong
cao hay
h cho
2015
Cao
trong
trong 7
c
. Trong 8
ra trong
imidacloprid
ph
Trong
azoxystrobin bao .
1-
dung
2.2.
3-
methanol,
Nam (
Cao
2015).
QUAN
CAO
HPLC di trao
pha
cao.
i ion hay
pha
h
(pha
6-
detector
hay
b
(HPTLC) Trong ng
in
2.2.3.1. HPLC bao
hai
cao
HPLC, i ta chia
pha
-
pha trao
ion
pha
trong
hay pha
tan
4 dung
dung ta
3 hai pha
HPLC 4
n
theo
tan ng.
dung
ta
cao (HPLC).
-
-
5-
8-
2.2.2.
-
syringe hay auto sampler).
7trong 2016)
t
cao
4-
2.2.1. Kh
pha
pha
2-
trong ngh
acetonitril,
dung
khi
4
4
2
ng
cho mong
theo kinh ta
i
c pha
pha
ng
tinh
t
nh. dung cho HPLC cho HPLC hay dung tinh
ghi pha
.
pha
0,2
hay
2013)
dung
m
qua Duy
100%. Tuy
pha
nhau.
o.
HPLC (
cao theo
ng dung
cho
p ion.
2.2.3.
dung m 1
ra
tinh 0,45
peak
c trong
2.2.3.2. i trong dung pha
trong
dung sau
-
pha
a peak thay
pha
y ra: dung
cho
i gian
i.
- Trong Pump
dung
e) khi
ng. Trong 2.3:
c
cho
HPLC 9
10
sai.
pha
t tan ra t (0
pha 0,5 2
m trong
ghi
+ Trong
cao
2.2.3.3.
qua
200 bar)
gian
ra
peak,
+
cho
peak trong
ng
theo
2.2.3.4. 2.2.3.8.
theo dung
a loop
5
100
2
trong
ng syringe)
in
Sau khi
li xong
pha
coi
tim
pha trong 1- 10 mm,
5 - 10
u
cao.
ng 10
30 cm,
tan trong
do
ra
theo
ra
Pha
(trong
t). c silan
USP 23, 24
ta
di
nhau
oxid, polyme
pha
Pha
qua
pha
theo pha
pha
nhau,
silicagel (pha (pha
bao
2016)
cho qua pha trong hay
tan
silicagel
in
trong
2.2.4.
2.2.3.5.
ra
ta
(auto sampler).
tan.
di cho
r
nh trao
Pha
theo
t
ion. cao
p
4
trao
trong
Trong .
T
2.2.5.
2.2.3.6. (hay cho
detector)
khi detector
-
chia
2
pha
Pha
theo
ghi
Thu, 2007)
pha
pha
g detector
cao khi
2.2.3.7.
pha
theo ta
An
cao
ra
ghi trong
nay, detector
ion
trong
cho
-
khi
quang cho
hay UV-Vis ko
Pha
pha
bao
mang silica 3 Pha
10
th
50 n theo
trong
ghi do detector 11
sang.
pha
Pha
c 12
h
mang
trong pha
-
Trong pha silica qua
silanol.
pha Pha Pha
trong ta dung
dung
thay
pha 2
pha
-
hay
dung
pha
thay
pha
,
ta chia
pha
pha
bao
pha pentan, hexan,
pha
Dung m
p
pha
pha
hydrocacbon pha
i
theo
2.4.
trong -
pha
pha tan
pha
2.2.6.2.
pha trong
trong dung
Dung
methanol, trong
pha
tan trong pha
tan qua pha
gian
Cs
mol
tan trong pha
CM
mol
ch tan trong pha
K ra
khi
cho
n khi
di
gian gian
K
(mol/l)
pha
pha
tan qua pha
g
nhau
h
tan.
K
trong ra
ng
n.
nhau t.
2.2.6.3.
gian
dung
dung
cho
trong hai
pha
pha
tan trong pha
pha
tan trong pha trong
tan. Trong
gian
pH
t
Trong hao gian
pha
Trong
peak
1-5
a ta
13
t R t0 t0
tR
gian dung
.
K'
.
ut
peak thay
(mol/l)
tR gian
theo
CS CM
An, 2007)
trong HPLC
gian
peak
K:
K
quan Trong
t
nhau gian
B
o.
2.2.6. 2.2.6.1.
A
K di
. pha
i gian
tR 14
2.2.6.4. (hay
gian
g
hai
A
RS
B)
hai
Trong hai
tRA, tRB:
hai
KA KB
A, B
tRA tRB
gian
Trong
nhau
1
2.2.6.5. trong trong H.
pha
c u
hai
pha
ng.
trung
t
B
ra
nhau
ta
AF Trong
a: n
(
sau peak
a
AF
b
1/10
1, peak
2
5,54
tR W0,5
peak. trong
2500
-
a
-
AS
5500
2.2.7.
ra hai peak
b
1/20
nhau
peak
peak trong
AS
1,5).
cho m:
Pha
sau: 15
0,8 - 1,5 (0,8
p ta bao
nhau theo
cao peak 1, peak
-
RS
g
a b 2a
As
gian
W0,5
cho.
cao peak)
AS
N
2.2.6.6.
b a peak
b: n
sau:
N
:
AF:
nh.
Trong
ra
pic pic
cao H
tR
RS hai peak
quan
trong
Trong
hai
t
pha
i
ra xa nhau, Do
H pha
theo
A
o
khu n
peak hai peak
cho (pha
2.2.6.7. thu
pic
RS = 1,5
R
hai
trong
nhau
peak
xa dung
nhau
tan trong pha
hai peak
RS = 1,0. Trong
nhau
nhau
cao
t RB t RA WB WA
. WB, WA:
KA KB
2
16
pha
-
pha
-
t.
Pha
u sau:
- Pha
ng:
pha
( pH,
isocratic. -
u
ch
pH,
- Pha
i
tan khi thay
phosphat
ngay
pha
hay
n
ta
pha
pha
-
l ta pha
2
pha
(NP)
ng (NP): Silicagel trung hay trung .
c OH
pha
alkyl
Pha
OH
ng (C8 hay C18 phenyl).
2.2.7.2.
thay
H
RP-8 hay RP-18) hay hay
c
pha
tinh
t
c
Trong pha ACN, MeOH, acid hay base
dung
trong
pha
(RP u
trong
RP- HPLC ra
ion carbon t t.
cho HPLC,
quang.
dung
ion.
alkyl
u.
amin hay acid amin -
c,
gian: gia
trong
dung
t
o (RP): Silicagel
m
i detector: detector UV-Vis dung acid acetic c < 220 nm). Detector
kinh HPLC), pha
c.
pha
carbon (phenyl-
quang
g
trong t.
cao: dung
nhanh
quang
(RP).
Pha
tinh
-
o
hay pha
theo trong
pha trong
dung
ACN hay MeOH
- Pha
u
pha
trong
dung
i gradient. 2.2.7.1.
cho pha
pH: 2,5 < pH < 8,5).
Khi
dung
pH. ta
v
E
dung
theo
sau: 2.3.
dung
trong u t
ta trong
pha
Dung
cho peak
i gian
dung
u,
. Pha
+ +
gian
+
n-Hexan
0,1
Tetrachlorua carbon
1,6
Toluen
2,4
Methanol
5,11
Acetonitril
10,20
gian thay
c
E
i:
t. i.
+ +
th t trong
peak.
Do
trong
pha
ta
pha
khi
p t
ta 17
18
nhanh
ta
cao.
c
tuy t
trong
gian, kinh
2.2.8.4.
. nhau 2012)
2.2.8. 2.2.8.1.
c
HPLC
-
theo
t,
cho
dung theo
dung khi cho
theo pha
c
ra. u
C
tra
theo
quy S
pha
c.
pha ch.
cho
hay khi
nghi
sau
dung
pha
ng a
NP-HPLC: R
RP-HPLC: khi pha l ACN hay methanol:
methanol; 50%: 50% cho
i trong
khi 100% sau
gian
c, N
dung
2.2.8.2. dung
pha
cho
tinh
tinh dung
t
theo
gian theo HPLC
2.2.8.3. X
theo
- Dung
, quy
tan
dung
pha
hay - Ph ra
h cho HPLC.
Pha dung
tan trong pha
theo
c sau:
trong
u
tan u. tan trong pha
t ly
qua
c 0,2
0,45 t.
t.
Pha dung
trong
dung ra
19
c sau: trong
t.
-
do
u
HPLC. Tuy
khi
20
3.
PH
STT
3.1.
Glassico
India
8
Neuburger
Germany
9
S100H Elmasonic
Germany
10
Balances and Precious USA Metal scales
7
dung
3.1.1. 3.1.1.1.
n
-
imidacloprid
azoxystrobin.
-
Sigma Aldrish
-
g: imidacloprid: 99,82% azoxystrobin: 99,60%
3.1.1.2. Dung 3.1. Danh m
11 dung
tinh
cho HPLC
cho HPLC 3.1.2.2.
STT
dung
1
Acetonitril
cho HPLC
2
Methanol
cho HPLC
-
3
hai
T
tinh 50 ml, 100 ml.
-
tia.
-
cho HPLC
vial
3.2. 3.1.2.
100 ml, 50 ml, 25 ml, 10 ml. 1 ml, 2 ml, 5 ml, 10 ml, 20 ml, 25 ml.
- Pipet
DUNG
-
imidacloprid
3.1.2.1
cao
3.2. Danh
-
cho -
STT 1
cao
2
cho dung
Pump
Germany
Vacuum Degasser
Germany
pha
pha
quy
3
Syringe
Hamilton
-
4
Injector
USA
-
5
Columns
Germany
hi nh
peak
-
RP-18, 250x4,6 mm,
6
ghi
azoxystrobin
sau:
UV/Vis Detector 21
Germany 22
imidacloprid
azoxystrobin
3.3. 3.3.1.
-
dung dung
pha
- Qua tham
-
, ,
ra dung
-
pha dung
pha
.
pha
dung c
RP
azoxystrobin,
i gian: 0
1
3.3.2.4.
Qua tham
ra dung
dung ra
ng
xu
pha
C8
C18
Tuy
m
danh
trong kinh
nay, p
m
so
tra,
ng.
ta
250 x 4,6 mm cho
RP
3.3.2.2.
18,
quan Do
u
detector UV-Vis
-
ng HPLC
imidacloprid
ta
t
: RP
18, 5
azoxystrobin
250 x 4,6 mm. 50 ppm.
1 C: acetonitril (CH3CN); D: n gian: 0 -20
3.3.
c
= 250 nm
thay
n pha
pha
acetonitril
Sau
HPLC
ng 220 nm, 250 nm, 255 nm, 260nm. UV-VIS SHIMADZU cho
hai
200-400nm
imidacloprid
thu
ra
(%)
Acetonitril (%) 95
10
90
5
85
15
80
20
azoxystrobin. tham
p 3.3.2.3.
nh
HPLC c 3.3.2.3 ta 23
t
20
pha sau:
ta
tham
gian
pha
- Detector: UV- Vis
i
c a
thay
nhau:
- Pha
g
thay
nhau
-
cho detector
Trong
thay
-
.
a HPLC, pha
pha kh
-
trang
ra pha
Khi pha thay
dung qua
ng
Trong
cho
2013)
t
t RP 18
ng
pha
pha
cho
t5
220 nm, 250 nm, 255 nm, 260nm. 20
.
3.3.2.1.
20 55%C: 45%D. 50 ppm.
-
dung
sau:
18, 5 m, 250 x4,6 mm.
- Detector: UV- Vis
dung imidacloprid
3.3.2.
HPLC
C: acetonitril (CH3CN); D:
-
cho
n
dung
t
- Pha
50 ppm
24
n
(gradient)
ng
(%)
Acetonitril (%)
peak (S), 60
40
55
45
50
50
40
(N) khi
6
gian
-
peak
-
3.3.2.5.
tan gian
peak, cho
pha
peak
trong
ra
0,8 - 1,5 (0,8
peak
trong
RP
50
dung
c
. 1
1,2
pha
tan
hay pha
dung
n imidacloprid
dung
azoxystrobin hai
.
:
= 250 nm. -
imidacloprid v
(ICH, 1996)
3.3.3.
1,5).
theo quy
dung
t; 0,8
- Detector: UV- Vis 20 -
AS
trong quy
sau 5
- Pha C: acetonitril (CH3CN); D: gian: 0 20 55%C: 45%D. 0,5
2,0%
3.3.3.2.
nhau.
18, 250 x 4,6 mm,
t
peak
1,5 (RS 1,5).
quy
ra
-
n
nhau
peak
-
1,0%
chung
HPLC quy
pha Tuy
(AS),
RSD > 2%, trong
C
pha
-
(RS),
2000.
RSD
-
(tR),
. t
-
60
gian
n
minh quy
u
Khi
t
y
-
pic
trong
sau dung
trong
-
y
2009)
3.3.3.1
6 25
ta
theo quy
pha
ng
.
tan
imidacloprid
dung
azoxystrobin hai
:
azoxystrobin cho
ch
hay pha
dung
dung n imidacloprid 50 ppm,
pic
2009) trong
tin
gian trong
gian ch
quy
sai
cho peak
dung
gian 1,0%, so
quy
azoxystrobin
gian
imidacloprid 26
azoxystrobin
Ghi
gian
peak
tinh
trong
x
- Ghi
.
peak trung
u.
Microsoft Excel 2003 v
quy
pic theo -
trong dung
cho peak peak
t
: peak
nhau
dung gian
gian 1,0%, so
0,997 (hay R2
ng quan (r)
nhau
i
gian
trong peak
trong peak
0,995).
r < 0,997
3.3.3.5.
peak
trung gian.
trong
- Peak
tinh
3.3.3.3.
LOD v
Trong quy (LOQ) hai
a ph
LOQ
c a h th ng s c
(LOD) quan
tuy n
h th ng s c K t qu
(LOD) cho h
c kh o
m t m u chu n h n h p imidacloprid
so
hay
v i
c peak
(RSD)
b ng
l pl i6l n
azoxystrobin
n ng
u ki n t i qua
S peak
c kh o
l ch chu n (SD), gian tR. RSD
(LOQ)
xem
RSD
trong 3 LOQ
5-7
- Pha 10 ppm -T
ta
imdacloprid dung
azoxystrobin RSD
pha
RSD 6 2,0%.
suy ra
3
ba pha ba dung
LOQ =
trong
80%, 100%
dung quy suy ra
10 × LOD 3
quan
theo
R%
quy
theo
hay
khi
20-160% i5
Mt 100 Ms
Trong
trong g
40%, 80%, 100%, 120%, 160%),
n
pha 5 3
- Ms : N
khi pha ( g/ml)
- Mt: N
( g/ml)
quy
cho -
HPLC
3.3.2 27
-
thu
6
trong
khi pha
ra
120% So
3.3.3.4.
dung
nhau
%)
3.3.3.6.
ghi k cao peak LOD
-
2,0%.
sau:
chu
HPLC
i
trung gian
hay LOD
m c 3.3.2. l ch chu n
2%,
so tr
n m trong kho ng
: 98,0% 102% cho quy 28
2,0 %
- RSD
4.
s
4.1.
3.3.4.
4.1.1.
dung
trong
Theo gian
dung
cao peak
quan
tan
Trong ta
quan
sau:
Hi = k1 . Ci = f(C)
(1)
Si = k2 . Ci = f(C)
(2)
pha
u
cao
n
Ci
peak
i
gian
Dung 10 mg, cho
i.
10 ml acetonitril,
ml,
400 ppm.
6 ml dung
- Dung xi
thu
qua
i 1
x1 x
imidacloprid Dung
2
n 1
RSD %
s .100 x
-T -L
khi
azoxystrobin.
p:
1 ml dung azoxystrobin
i 1
dung
0,45 50 ppm.
Dung -
SD
cho
acetonitrile
n
n
imidacloprid
pha
- H
theo p
1 n
ch
Dung
(1) (2) ta hay x
hai
azoxystrobin. Dung - Dung dung
tRi.
25 ml.
10
acetonitril
t pha
trung
dung
-
k1 , k2
a
dung
trong pha
Si
trong acetonitril
acetonitril dung
Trong Hi
pha
dung
imidacloprid 50 ml.
5 ml dung
acetonitril qua
0,45
imidacloprid
khi
azoxystrobin
Dung 50 ppm.
4.1.2 K Sau khi
theo
3.3.2, ta thu
sau: cho detector
4.1.2.1.
detector
quan nh sao cho
ta
200-400 nm sau: 29
30
thu
50
1.500
azoxystrobin
1.000
Abs.
imidacloprid 0.500
0.000
-0.500 200.00
4.1:
250.00
th
4.1 cho
300.00 nm.
a azoxystrobin
350.00
imidacloprid trong acetonitrile.
azoxystrobin
thu
imidacloprid
c
270 nm. Hai
nhau hai
400.00
250 nm.
207 nm, thu giao
ACN/
(90%:10%).
4.3.
ACN/
(95%:5%).
pha
4.1.2.2. pha 3.3.2 imidacloprid dung
4.2.
250 nm
thay azoxystrobin
c pha pha
pha
Dung dung
chu c 400 ppm.
h
acetonitril
nhau. pha trong
c 3.3.2.4.
t
sau:
31
32
4.4.
4.5.
ACN/
ACN/
(85%:15%) 4.6.
ACN/
h 4.7.
ACN/
(55%:45%).
(60%:40%). (50%:50%).
4.2; 3.3; 4.4; 4.5; 4.6; 4.7, ta
pha
gian ACN
(80%-95%)
pic
gian , peak
nhau cao
nhau, .
, n.
peak imidacloprid
pha nhau (55%:45%) cho 33
a peak. hai
h dung
ACN theo.
34
ra khi ta
t
ng
4.1.2.3 c imidacloprid
azoxystrobin
nhau:
0,5 0,8 1 ml 1,2 1,5 sau: -
t
RP
18,
-
250 x 4,6 mm.
u: 20
t 50 ppm - Detector UV-Vis: 250 nm. - Pha
pha
3.3.2.4. theo
c 3.3.2.5. Theo
ta
qua 4.8:
gian -
0,6
0,8
cho
i gian
4.1.
n, peak
ng
imidacloprid
nhau -
1
tR
cho
nhau
,
-
Do
ta
4.2.
hao gian d
dung peak
1
ng
NG
4.2.1.
As
Rs imi
N
1
3,954
626144
1,140
0,941
0,00
39194,789
2
3,949
634100
1,126
0,955
0,00
39100,101
3
3,969
638942
1,138
0,967
0,00
39103,700
4
3,947
642210
1,156
0,942
0,00
38679,280
5
3,974
643648
1,162
0,951
0,00
39004,980
6
3,960
660550
1,128
0,960
0,00
38243,829
Trung
3,957
640932
1,142
0,953
0,00
38887,780
%RSD
0,309
1,797
1,282
0,011
0,00
0,933
SD
0,012
11517
0,015
0,0101
0,00
362,722
ra
imidacloprid.
IMIDACLOPRID
x
.
(> 1
azoxystrobin
Speak
HAI AZOXYSTROBIN quy
4.2.1.1. Pha dung
azoxystrobin 6
35
imidacloprid
50 ppm.
36
4.2.
ng azoxystrobin Speak
tR
x
As
Rs azo
4.2.1.2 N
1
12,058
1805578
1,013
2,012
2,056
76407,704
2
12,081
1814130
1,009
2,212
2,059
75540,833
3
12,165
1824734
1,007
2,411
2,065
75960,530
4
12,072
1832351
1,021
2,254
2,059
76049,748
5
12,215
1835474
1,014
2,211
2,074
76593,872
6
12,144
1828874
0,999
2,231
2,067
73276,171
Trung
12,122
1823524
1,010
1,889
2,063
75638,143
%RSD
0,513
0,631
0,731
21,12
0,315
1,605
SD
0,012
11498
0,0073
0,399
0.0065
1213,992
hai gian (AS)
(tR), trong
4.1
4.2 cho
peak (S), ng 0,8-1,5,
4.9:
2%, (RS)
imidacloprid
azoxystrobin
cho
1,5, -
theo
pha
gian c
dung
imidacloprid azoxystrobin. - Trong
pha
azoxystrobin trong trong
dung
a
hai peak
gian
imidacloprid
pic azoxystrobin.
1 peak
uk
gian imidacloprid
pic c
a imidacloprid
imidacloprid gian
nhau
azoxystrobin n n trong s
peak
peak azoxystrobin
pic
peak imidacloprid
2,606 trong azoxystrobin
azoxystrobin:
. Peak imidacloprid
to cho
dung azoxystrobin
rang
hai peak imidacloprid gian
3,959
37
12,210 peak
38
gian
imidacloprid
-
azoxystrobin
,
cho hai peak
azoxystrobin
imidacloprid
g
dung
T
a imidacloprid
- LOD peak
suy ra:
gian
- LOQ
a azoxystrobin =
10 10 LOD = x 0,048 = 0,16 ppm. 3 3
- LOQ
a imidacloprid =
10 10 LOD = x 0,0048 = 0,016 ppm. 3 3
quy
4.2.1.3.
LOD
LOQ
quy Trong (LOQ) hai
h quan
LOD chu dung
4.2.1.4. a imidacloprid
ta
imdacloprid pha
cao peak = 3
(LOD)
ng.
LOQ
sau: pha
azoxystrobin
5
10 ppm
Sau y
pha
t
dung
n
khi
pha
LOD
n
- Pha
dung
imidacloprid
50 ml
1,6 ppm:
- Pha
azoxystrobin
0,048 ppm
sau: 0,4
azoxystrobin 40 ml dung
ng acetonitril cho dung 10 ml
cho 4.3: khi
n
40%, 80%, 100%, 120%, 160%.
sau:
50 ml,
p imidacloprid
azoxystrobin
0,4-1,6 ppm
ppm; 0,8 ppm; 1 ppm; 1,2 ppm; 1,6 ppm
HPLC.
cao
7
2 ppm
4.10:
0,0048 ppm.
pha
ch 1,6 ppm
ch
thu ng acetonitril.
dung HPLC
Vx ml sau:
imidacloprid
azoxystrobin
C(ppm)
0,4
0,8
1
1,2
1,6
Vx ml
2,5
5
6,25
7,5
10
Vacetonitrile
c
Sau
cho
.
n
HPLC
c
sau:
-
t
RP
18, 250 x 4,6 mm,
- Pha
C: ACN 55%; D: N
c: 45%
pha ng: 1 - Detector UV-Vis: = 250 nm. 4.11.
imidacloprid 4.10
imidacloprid - LOD
0,0048 ppm a azoxystrobin
azoxystrobin
4.11 cho
khi
cao = 3 0,048 ppm 39
u: 20
0,0048 ppm azoxystrobin
n
0,048 ppm
pic S
C
.
pic S thu
quy
n
n.
Do
ra trong ghi
a
Microsoft Excel 2003 40
ng,
, quy.
4.4.
peak
imidacloprid trong
Imidacloprid C (ppm)
Speak
0,4
81789
0,8
152152
1
226200
1,2
291980
1,6
368627
4.5.
peak
azoxystrobin trong
4.12.
peak
imidacloprid
4.13.
peak
azoxystrobin
ch
azoxystrobin C (ppm)
Speak
0,4
185609
0,8
357070
1
506195
1,2
670685
1,6
870305
ta trong
41
4.12, 4.13
4.4
quy sau 4.5.
42
4.6.
quy
azoxystrobin
imidacloprid
4.8.
th gian
quy
quan R2
(ppm)
HPLC
u imidaclopid
imidacloprid
peak
imidacloprid
TT gian
imidacloprid
R2=0,9978
Y=74105x
azoxystrobin
0,4-1,6
2
Y=171865x
R =0,997
Qua
ta
imidacloprid
0,4
1,6 ppm. Do
hay
3,964
trung
2360311
Xtb=3,959
Xtb=2383429,5
quan hai t
3
3,971
4
3,966
imidacloprid trong
5
3,973
6
3,922
2339617
SD=0,0188
2375992
SD=34611,11
ta
ng azoxystrobin
u
2
2375675
trung
peak
c 3.3.3.4.
azoxystrobin
3,959
0,4-1,6
nhau cao
1
.
2419586
RSD(%)=0,47%
2429396
RSD(%)=1,45%
4.2.1.5. Theo p6 p azoxystrobin u
c 3.3.2. (RSD)
imidacloprid
peak
4.7.
qua Speak
HPLC gian
gian
peak
2
12,077
3
12,132
4
12,167
5
12,205
6
12,311
trung Xtb=12,162
6472807
G
6535964
Xtb=6495348.67
6419486
peak 1
2
3
1
2367836
2341037
2352453
2
2301897
2401004
2390451
3
2401211
2390312
2385421
4
2315012
2352789
2410207
5
2342202
2321107
2331652
SD=60348.26
6
2296789
2321775
2314473
Trung
2337491
2354671
2364109
2352090
1,75%
1,44%
1,57%
1,59%
RSD 6592855
43
imidacloprid
trung
6475006
RSD(%)=0,72%
trung gian
azoxystrobin
6475974
SD=0,088
imidacloprid
trung gian 4.9.
gian 12,081
n pic 0,92 % 3.3.3.5. Quy .
(SD), tR .
TT
1
ta
HPLC
u azoxystrobin
azoxystrobin
ng, azoxystrobin
RSD(%)=0,92%
44
1,45 %
4.10.
trung gian
azoxystrobin
2455806
250
248,79
101,00
2505612
250
254,83
98,12
3
2502276
250
254,13
98,25
2927766
300
306.12
98,00
2865312
300
298,53
100,30
2887210
300
301,20
99,60
peak 1
100%
2
1
6399178
6417754
6475441
2
6400153
6438765
6390435
3
6403347
6443221
6485421
4
6421182
6432119
6410379
5
6501122
6421277
6478553
6
6467781
6456423
6455763
120%
ng 4.12.
s Azoxystrobin pic
(%) Trung RSD
%
6432127
6432927
6449332
6438128
x
0,66%
0,23%
0,61%
0,5%
4860132
200
202,03
98,98
4788941
200
201,51
99,25
4888295
200
203,50
98,28
5804669
250
250,52
99,79
5898400
250
259,31
98,41
5870421
250
253,89
98,46
6779319
300
300,51
99,82
6698359
300
296,36
101,22
6700758
300
296,48
101,48
thu
theo
cao (RSD
4.9 peak
4.10 cho
80%
quy
2%).
quy
hai
imidacloprid
azoxystrobin
HPLC
cao, do
100%
quy 4.2.1.6. 4.11.
Imidacloprid
120%
Imidacloprid
t imidacloprid
pic
(%) x
80%
i azoxystrobin
quy
3
azoxystrobin
trong
trong
4.9
4.10 c
ng 98-102%
% quy
2050270
200
199,50
101,00
2082793
200
203,46
98,29
2054821
200
200,06
99,97
45
quy
ng imidacloprid
HPLC
azoxystrobin t
46
4.3.
5. HPLC:
5.1. K trang
Tuy
cao, dung
qu
HPLC
so khi
.
u
trong
cao: t cho
-
,
trong
azoxystrobin trong h cao cao.
-
sai
HPLC
Nam. Nam
Trong s
RP
18; 250 x4,6 mm;
- Pha
acetonitril:
-T
g: 1
-
imidacloprid
(55%:45%)
20 c
g: 250 nm sau: C
cho chung
hai
RSD
quy
chi
Imidacloprid
1,45%
0,92% nh
quan )
quy trong
0,997 (hay R2 0,995) 98-102% quy
hai trong xu , trong
5.1: azoxystrobin
. Trong g
tham hai
azoxystrobin
. gian,
.
azoxystrobin
trong
peak
trong .
c, dung
RSD
hai
azoxystrobin.
t,
cho peak imidacloprid
Qua
Quy
peak
gian
azoxystrobin
HPLC
LOD, LQD
IV
quy
cao, .
n
cho 2
imidacloprid
imidacloprid
azoxystrobin
LOD (ppm)
0,0048
0,048
LOQ (ppm)
0,0016
0,016
Y=74105x
Y=171865x
hai . Do
5
cho
quy
imidacloprid
c detector UV-Vis.
- Th
HPLC
. Do .
trong
imidacloprid
trong h
t. gian, dung
-T
azoxystrobin n sau:
ch
:
-
imidacloprid cho
cao
quy quan
2
R =0,9978
R2=0,997
0,4-1,6
0,4-1,6 ,
trang 47
cao
, dung 48
, quy
,
THAM
5.2. thu t
ta
gp HPLC cao, imidacloprid azoxystrobin
cho HPLC
trong
.
c ra
Thay
thay
hai
dung
Thay
imdacloprid
azoxystrobin
Y 7
(2009),
2.
sau: gian
1.
hao
dung
Minh
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chung cho
g trong quy
h trong
u
quy
Dung (2014).
4.
Hi trong trong
(2014).
quy
Y
dung
RP - HPLC
ASEAN v 22/2009/TT-BYT Quy
trong
5.
(2015).
fluconazol
.L
ra. 6.
.
Minh. Duy Cao
quang
UV VIS
(2015).
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s
8.
An
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An
(2007).
. NXB Y Thu (2007). . NXB Khoa
(1995).
11.
(2016).HPLCY
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TP.
(2003).
cao (HPLC) 7.
Y
,
II, NXB Y , , .
trong
.
Minh. (2013). s
Calci Atorvastatin cao.
Simvastatin
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52
12
1:
Imidacloprid
1.3. 1.1.
imidacloprid C= 80ppm, 1.1 Speak
5,425
x
226144
1.2.
1.3 tR
sau:
As
Rs
1,100
0
imidacloprid 1.2
tR
3,959
Speak
x
386504
(50%:50%), sau:
255nm
4,683 tR
imidacloprid
(60%:40%),
N
0
19094
(55%:45%), sau:
As
Rs
1,208
0
N
0
26076
nm
Speak
x 3702019
As
Rs
0,652
0
N 0
29705
nm
2.2
Azoxystrobin
2.
tR
Speak
5,179
2.1.
Azoxystrobin
(55%:45%), 2.1
Speak (
tR 12,164
x
1805578
Rs
N
0,813
2,011
2,043
46709
sau:
As
Rs
1,013
0
N 0
2.3.
Azoxystrobin v
66407,502
(80%:20%),
nm
(60%:40%), 2.3
5,179
Azoxystrobin
1705578
As
nm
tR
2.2.
x
sau:
Speak
x 1705578
nm
sau:
As
Rs
0,813
0
N 0
46709
3.
azoxystrobin
imidacloprid
3.2. 3.1.
azoxystrobin (55%:45%), 3.1
azoxystrobin
imidacloprid
3.2
nm sau: tR
tR
Speak
x
As
Rs
imidacloprid
(55%:45%),
Speak
x
nm sau: As
Rs
N
N
imidacloprid
3,949
616204
1,140
0,941
0,00
39194,789
azoxystrobin
12,081
1814130
1,005
2,231
2,05
75530,733
imidacloprid
3,963
529831
1,140
0,941
0,00
37634,532
azoxystrobin
12,143
1795231
1,315
2,511
2,12
75820,611
NAM KHOA
-
-
do -
B
sinh
THEO
: 7B
MSSV: 3.3.
azoxystrobin
3.3
quy
imidacloprid
(60%:40%),
12D720401175 l
imidacloprid
azoxystrobin
nm
n ng ThS.
sau: theo
tR
Speak
x
As
Rs
sau:
N
:
1. imidacloprid
3,953
629732
1,140
0,941
0,00
39600,411
azoxystrobin
12,103
1895321
1,315
2,471
2,33
69947,623
sau
hai
tham
tham l
tham
2.
website theo
quy
sung ra,
trong
dung :
quy
imidacloprid
azoxystrobin
d
quy
imidacloprid
azoxystrobin
n ng sung dung sung imidacloprid
t
trung gian.
azoxystrobin trong pha
dung trong
sung tham
trong
SINH
PGS.TS