THNG QUY K THUT

XAC NH MT S HOA CHT BO V THC VT (HCBVTV)

NHOM LN HU C BNG PHUNG PHAP SAC KY LP MONG
VA PHUNG PHAP SAC KY KHI
1. Nguyn tc
Du luong thuc bao v thuc vt gc ln huu co duoc chit tach khoi mu
bng axeton. Sau do lam sach bng cach cho qua ct Ilorisil. Ban dinh
luong hoa cht bao v thuc vt bng sc ky lop mong sau khi d hin mu
bng nitrat bac hoc dinh luong bng sc ky khi voi Detector ph ngon lua
(FPD) hoc Detector nito photpho (NPD).
2. Pham vi ap dung
Phuong phap nay ap dung d xac dinh luong tn du cua mt s hoa cht bao
v thuc vt nhom ln huu co trong rau qua, ngu cc, che, ca ph.
3. Dung cu, hoa cht, thuc thu
3.1. Dng c, thit b
- May nghin mu
- May lc.
- May ct quay chn khng hoc b ct cach thuy.
- Bom chn khng.
- Binh cu 150 ml, 500ml.
- Binh tam giac 300 ml, 500 ml nut mai.
- Binh dinh muc 10 ml, 50 ml, 100 ml.
- Binh chit dung tich 250 ml.
- Binh sc ky: rng 5 cm, cao 25 cm, dai 25 cm.
- Ban mong 20 x 20 cm loai silicagel 60 trang sn: dung thuoc ke va but chi
chon danh du vach xut phat cach mep duoi 1,5cm va cach hai canh bn
ban mong 0,5 cm d tranh hiu ung bo.
- Binh hut m duong kinh 25 cm.
- ng dong 10 ml, 50 ml, 100 ml.
- Binh gan 500 ml.
- Ct sc ky co khoa 00 x 20 mm.
- Phu hut chn khng.
- Binh phun suong thuc thu.
- Micro syringe.
- en tu ngoai UV.
- May sc ky khi.
3.2. Ho cht
- Cac cht chun cua HCBVTV: Methyl parathion, Diainon, Malathion,
Dimethoat, Dichlorvos.
- xeton (TKPT)
- n - Hexan (TKPT), n - Heptan (TKPT)
- Natri sunIat khan (TKPT)
- Cn etylic ( TKPT).
- Bng thuy tinh.
- Bac nitrat (g NO
3
) (TKPT).
- moni hydroxyt dm dc (TKPT).
- Natri clorua (TKPT)
- te etylic (TKPT)
- te du hoa (TKPT) phn doan 0-60
0
- Florisil: cn khoang 20g Ilorisil cho vao tu sy, sy 650
0
C trong gio
sau do sy qua dm 130
0
C. ngui va thm khoang 0, ml nuoc. Nhu
vy ta duoc Ilorisil giam hoat tinh 2.
3.3. Chun b thuc th, dung dch chun, dung mi
3.3.1. Chun bi h dung mi khai trin:
Hn hop n Hexan: axeton 2:1. Cho 0 ml n - Hexan va 20 ml axeton trn
du va rot vao binh trin khai sc ky, dy np binh lai.
3.3.2. Chun bi dung dich thuc hin:
Cn 0, 5g bac nitrat cho vao binh dinh muc 100 ml. Thm 5 ml nuoc ct hoa
tan hoan toan luong bac nitrat. Thm 5 ml amoni hydroxyt dm dc va b
sung axeton dn vach muc, lc du. Bao quan trong tu lanh han su dung 10
ngay.
3.3.3. Chun bi dung dich chun:
- Chun : Cn 10 mg mi loai HCBVTV chun, cho vao trong binh dinh
muc 100 ml, dinh muc bng axeton dn vach (dung dich chun ).
(chun co nng d:100 mg ml dung cho phuong phap ban mong).
- Chun B (dung cho phuong phap sc ky khi):
Dung dich HCBVTV (chun B): Dung pipet chinh xac hut 1ml dung dich
chun cho vao binh dinh muc 100ml, thm axtn dn vach muc (Chun
B co nng d mi loai 1 mgml).
- Cac dung dich chun bao quan diu kin lanh duoi 0
0
C.
. Phuong phap tin hanh
4.1. Chun b mu
Cn 50 g mu d duoc nghin nho du cho vao mt binh tam giac nut nham
500 ml, thm vao do 200 ml axeton lc trn may lc hoc bng tay trong
vng 30 phut. Loc mu qua binh co phu loc chn khng. Sau do trang lai
mu va phu bng 30 ml axeton. ot toan b dich loc sang binh gan th tich
1lit, thm vao do 30 ml dung dich mui natri clorua bo hoa va 300 ml nuoc
ct. Chit xut hn hop trn voi n - Hexan hai ln mi ln 50 ml. lng
gan rut ly phn dung mi huu co n -Hexan vao mt binh non qua phu thuy
tinh co chua Na
2
S0

khan d loai nuoc.

Ct quay chn khng dung dich n -Hexan va thu duoc hoc cach thuy
nhit d nho hon 60
o
C toi khi dung dich cn khoang 10 ml.
!m "#ch mu$
- Lot duoi day ct sc ky co khoa mt lop bng thuy tinh va khoa vi lai.
ot dy ct dung mi rua giai 15 ete etylic trong ete du hoa ri d dn
vao cac ct sc ky Ilorisil d giam hoat tinh sao cho Ilorisil nhi du vao ct.
Trn mt phu mt lop Na
2
SO

khan. M khoa d dung dich rua giai chay ra,

trang lai ct bng mt luong dung dich rua giai nua sao cho ct khng bi
kh (k t lop Na
2
SO

khan). ot dung dich mu thu duoc trn vao ct va

sau do rua bng 200 ml dung mi rua giai 15 ete etylic trong ete du hoa.
Dung dich rua giai duoc thu vao binh trn, dem ct chn khng quay trn toi
cn kh. Hoa cn (mu phn tich) vao 1 ml n - Hexan.
4.2. %in h!nh &'t nghi(m
.2.1. Xac dinh bng sc ky lop mong:
Dung micro syringe ly chinh sac 2 5 10 20 ml dung dich chun va dung
dich mu chm ln ban mong, mi vt chm cach nhau 1 - 2 cm. Chm xen
k vt mu thu va vt chun d sau khi hin mau co th so sanh va nhn xet
kt qua (dung micro syringe ring cho tng loai nng d dung dich chun va
dung dich mu). co kt qua tt cn chm sao cho vt chm cang nho cang
tt. Ban mong sau khi chm, lam kh, dt vao binh sc ky va dy np lai.
Cn bo hoa binh sc ky truoc khi chay bng cach d 5 ml dung mi chay
sc ky vao binh, dy np va d trong 30 phut. Bo hoa binh truoc s lam
giam thoi gian chay sc ky va tng tinh dng nht cua
I
. Khi dung mi trin
khai ln dn cach mep trn khoang 1,5 cm, ly ban mong ra, d bay hoi dung
mi trong tu ht. Phun dung dich thuc hin mau bac nitrat. t ban mong
duoi den tu ngoai UV 365 mm t 15 dn 20 phut, nn ban mong den dn.
Vt sc ky cua cht s hin ra mau vang nhat dn nu nhat.
So sanh vt thu va vt chun co cung
I
d dinh tinh duoc vt do trong mu
thu.
So sanh cuong d hunh quang: Vt mu nao co cuong d hunh quang
bng cuong d hunh quang cua vt chun thi mu co nng d bng nng d
cua vt chun do.
Cac gia tri
I
trung binh cua cac cht:
Gia tri
I
cua cac vt:

I

h
x
h
dm
Trong do:
h
x
la khoang cach cua vt trong mu chay sc ky ban mong
h
dm
:

la khoang cach dung mi chay sc ky ban mong
Diainon 0,30
Dimethoat 0,3
Dichlorvos 0,5
Malathion 0,61
Methyl Parathion 0,66
nhy cua phuong phap di voi Methyl parathion, Malathion la 1 mg
trong vt. i voi Dimethoat, DDVP, Diainon la 5 mg trong vt ban mong.
Mau sc cua vt co th hin thy mt cach r net nht khi trong vt chm co
trn 15 mg du luong HCBVTV.
.2.2. Xac dinh bng phuong phap sc ky khi:
iu kin lam vic:
Ct sc khi ky: Su dung ct mao quan SPB-1, kich thuoc 30m x 0,25 mm x
0,25 mm (hoc cac ct tuong duong).
- Khi mang: Heli tinh khit ,
- Detector: FPD hoc NPD.
- Khi dt Hydr: Tinh khit GC
- Khng khi nen: Tinh khit GC
- Nhit d ct: Theo chuong trinh
20
o
Cmin 5
o
Cmin
50
0
C (1 min) a 120
0
C a 20
0
C
- Nhit d detector: 300
0
C
- Luu luong khi mang: 0, mlmin
- Phuong phap bom mu: khng chia dng, 2 minchia dng
- Nhit d bung bom mu: 250
0
C.
- Luong mu bom: 2 ml.
- Luong mu chun bom: 2 ml chun B (muc 3.3.3).
Tinh kt qua:
- So sanh thoi gian luu cua mi dnh so voi dnh cht chun d dinh tinh.
- So sanh chiu cao (h) hoc din tich cua mi pic (S
m
) voi pic cht chun
tuong ung (S
i
) d tinh dinh luong.
Ham luong HCBVTV tng loai duoc tinh theo cng thuc:
X
i

S
i
x C
i
x V
S
m
x m
Trong do:
X
i
- Ham luong HCBVTV cht i co trong 1 kg mu (mg kg)
S
i
- Din tich cua pic tuong ung mu phn tich co cht i (mm
2
)
S
m
- Din tich cua pic tuong ung mu chun co cht i (mm
2
)
C
i
- Ham luong cht i co trong 1 ml dung dich chun (mg ml)
V - Th tich dich chit mu cui cung (ml).
m - Khi luong mu ly phn tich (g).
Ghi chu:
4.3. Hi(u "ut thu h)i c*+ ,h-.ng ,h,$ 2 5
- nhy cua phuong phap: 0,01 mg kg.
- Sai s trung binh cua phuong phap: 15.
- Thoi gian luu cua mt s cht:
Tn HCBVTV Cng thuc hoa hoc Thoi gian luu (phut)
Metamidophos C
2
H

NO
2
PS .0
Dichlorvos C

Cl
2
O

P .5
thoprophos C

H
1
O
2
PS
2
1.5
Dimethoate C
5
H
12
NO
3
PS
2
16.0
Diainon C
12
H
21
N
2
O
3
PS 1.5
Methylparathion C

H
10
NO
5
PS 1.5
Malathion C
10
H
1
O
2
PS
2
21.5
Chlorpyriphos C

H
1
Cl
3
NO
3
PS 22.0
ChlorIenvinphos C
12
H
1
Cl
3
O

P 23.0
uinalphos C
12
H
15
N
2
O
3
PS 23.5