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PHN TRNH BY
I. NHNG S KIN V AN TON THC PHM
II. CC HA CHT C HI
III. NHNG THCH THC TRONG PHN TCH
KIM NGHIM M BO AN TON THC PHM
I. NHNG S KIN
1.Cung cp thc phm (TP) hin nay mang tnh ton cu i hi phi
tng cng gim st m bo an ton thc phm (ATTP)
2. Thc phm hin rt nhiu v phc tp, ph gia thc phm rt a dng,
an xen vi ha cht c kh nng gy c c tnh hay do thiu hiu bit c
cho thm vo to c mt c trng nhm t li nhun bt chnh
3. Mc nguy him c th rt ln i vi nhng thc phm sn xut ti cc
nc c h tng cha tht pht trin v c cu gim st cha tht hiu qu
Cc mi nguy him: vi sinh, vt l, ha hc, hng nhi
4 Mt chuyn ngnh gi l Foodomics
chuyn nghin cu thc phm
(dinh dng, thc phm bin i gen, protein hc, c cht hc lin quan)
Trong nhng nm gn y, hng ho Vit Nam xut khu nhn chung c cht
lng tt hn nh cc bin php qun l cht ch, h thng phng kim nghim
ngy cng c tng cng v hot ng c hiu qu
H THNG THNG BO V CNH BO CA CHU U V CHT LNG
THC PHM CHO NGI V THC N CHN NUI
Nm
S l hng khng t
yu cu
Th
hng
Nm
S l hng khng t
yu cu
Th hng
2002
67
2007
45
18
2003
19
35
2008
56
15
2004
59
13
2009
100
11
2005
124
2010
71
13
2006
68
13
2011
109
*Vic gi nhn hiu, vic s dng nhng ha cht nhi ph gia TP c th nguy
hi cho sc khe ngi tiu dng, v mc ch li nhun phi php, to nhiu vi
phm v ATTP:
-melamine trong sa v sn phm t sa, ng cho vo mt ong
-DEHP dng lm cht to c, phm mu cng nghip b cm dng trong TP,
-nc tng nhim 3-chloro-1,2-propandiol (3-MCPD)
- phm mu cng nghip rhodamine B nhum ht da, 2,4-diaminoazobenzene
dng nhum g vt cho c mu vng ti, orange II nhum tht quay v tht x xu
cho c mu cam ti bt mt .
-khng sinh, cht dit nm mc trong nui trng thy sn,
-ha cht tng trng b cm: clenbuterol v salbutamol, ractopamine , to tht siu
nc trong chn nui gia sc gia cm
-trifluralin trong thy sn v ethoxyquin trong tm do b nhim t thc n.
SO NGI
CHET
1997-2000
1391
25 509
217
2001
245
3 901
63
2002
2005
2006
2007
2008
2009
2010
2011
2012 (n 12/2012)
208
144
165
248
205
152
175
148
164
4 894
4 300
7135
7329
7828
5200
5664
4700
5400
71
53
57
55
61
35
51
27
33
CHI PH/NM
Agilent GC-MS/MS
KHNG SINH
ACRYLAMIDE
3-MCPD
DEHP
MELAMINE
BIS PHENOL A
Acrylamide
OC CHAT DE SINH RA T CACH CHIEN, XAO NNG LAM THC AN CUA
TA.
HAM LNG ACRYLAMIDE AC BIET CAO TRONG KHOAI TAY CHIEN.
IARC SAP ACRYLAMIDE VAO LOAI CO KHA NANG GAY UNG TH CHO NGI (Class
2A, LD50 chuot 107/mg/kg the trong).
[g/kg]
min.
max.
Trung
bnh
[g/kg]
Hm lng
Thng gp
So mau
nhiem
Khoai chin lt
mng
192
140
3640
819
1000
76
98
< 10
2779
151
570
11
38
< 10
1090
190
660
C ph bt
30
115
1685
343
370
14
Bnh m nng
ming nh
32
15
1714
133
610
Ng cc n sng
32
< 10
846
65
260
Asparagine
Nhit, ng
(glucose, fructose)
Acrylamide
DEHP
O
DBP
CH2 CH3
C O CH CH (CH ) CH
2
23
3
C O (CH ) CH
23
3
C O (CH2)3 CH3
DBP : my pham
QUI NH NAY CUNG C VIET NAM AP DUNG (QUYET NH 3339/2001/QBYT NGAY 30/7/2001).
TUY NHIEN, TRONG DANH SACH CAC HOA CHAT CO THE THOI RA TH
OI VI ESTE PHTALAT, VIET NAM CH LIET KE DIETHYL PHTALAT.
O
C
Di(2-ethylhexyl)
phthalate (DEHP)
C
O
CH2CH3
OCH2CH(CH2)3CH3
OCH2CH(CH2)3CH3
CH2CH3
Bisphenol A, ha cht c c th
thi ra t cc binh sa
N N
NH2
H2N
Orange II
Tht heo quay, x xu
2,4-diaminoazo
benzene
g, vt ti sng
Rhodamine B
ht da
Para Red
gia v, mt s loi ht
III.1. CHUN BI MU
Chit cht phn tch
(Extraction)
Mc ich:
Lm m c v tinh ch
loi tp (Clean- up)
nh lng
GC-MS; GC-MS/MS
LC-MS, LC-MS/MS
H QU
* Sc km cht lng
* Kh khn trong nhn danh cht phn tch
* Gim nhy khin khng phn tch c lng nh cht
* Gim kh nng to ion t cht phn tch, nht l u to
ion ESI, dn n nh lng sai nu khng c bin php ph
hp
* lm bn h my phn tch, gy nght ct.
Hot ha
Np mu
H Combi-Pal
Ra loi tp Ra gii
Gn nh khng chun b mu
Vtng
ml
Cchunthm
ppm
Cng
mi sc k
Vnc
l
VMeOH std
l
Cstd
ppm
0.5
80
30400
0.58
0.00
1254132
0.5
70
10
30400
0.58
524.16
2230763
0.5
60
20
30400
0.58
946.71
2809327
0.5
40
40
30400
0.58
2096.55
4707576
Ct ng chun
(ppm)
795.91
5000000
Area
4000000
3000000
2000000
y = 1629.6403x + 1297053.7546
R2 = 0.9986
1000000
0
-1000
1000
2000
3000
C (ppm)
Mu C, i chng
Mu B
Dy hydrocarbon chun
C13
C14
C15
C16
C17
Mu B
C13
C14
C15
C16
C17
C18
Mu D
C12
C13
C14
C14
C15 C16
Mu E
C12
C13
C17
Nguyn tc
Phng php EZ:faast nguyn thy c p dng cho phn tch aminoacid.
Aminoacid trong mi trng acid c cho qua v gi li trong mt u lc
cha nha trao i cation, sau c n vo mt vial thy tinh v c
chuyn ha nhanh bng n-propyl chloroformate trong chloroform. Sn
phm chuyn ha c chit khi mi trng phn ng bng isooctan . Mt
lng dung dch c em thi kh di N2 v nh mc li bng pha ng
, lc v tim vo my LC-MS/MS.
SO3 H
+ R
CH
NH3
COOH
u lc SCX
SO3
H3N
CH
COOH
Ra vi nc kh ion
SO3
H3N
NaOH
CH
Ra gii
COOH
SO3 Na
CH
COO
NH2
RCH
NH2
COO
Cl
CH2CH2CH3
Chuyn ha
O
Cl
CH2CH2CH3
CH COOCH2CH2CH3
NHCOOCH2CH2CH3
Isooctane
Sn phm chuyn ha
Conc. of A
(mg/L)
A/512
A/128
A/64
A/16
A/8
A/2
Phenethylamine
23.776
11137
43830
98330
356097
721678
2843597
Tryptamine
24.057
161497
665310
1239572
4729615
9534987
35716484
Putresceine
24.746
220446
883123
1633455
6632519
13265038
52943154
Cadaverine
47.134
569946
2263573
4533683
18881438
38013484
140317910
Histamine
10.094
91637
365599
770881
2681246
5406498
20467821
Tyramine
18 334
346657
1373636
2910502
12072790
24975146
98137104
Spermidine
12.375
20349
81682
184494
644621
1304684
5097514
Serotonine
15.741
94037
372146
683018
2948357
5913565
21551005
Spermine
28.906
22219
90016
194243
786734
1590137
6005443
BA
R2 = 0.9999
R2 = 0.9997
R2 = 1.000
R2 = 0.9995
R2 = 0.9998
R2 = 1.000 .
R2 = 0.9999
R2 = 0,9993
R2 = 0.9998
Sc khi ca mu nc mm M4
Phenethylamine
Histamine
Tyramine
Putresceine
Spermidine
Tryptamine
Serotonin
Cadaverine
Spermine
2. Ly tm 2 3 pht
5. Cho vo LC-MSMS
4.Ly tm 2 3 pht
5. Cho vo GC-MS
K THUT QuEChERS
K thut QuEChERS
*Lm n gin ha khu chun b mu so vi truyn thng
*Rt it tn thi gian
*Ph hp vi ha phn tch xanh
-khng i hi thy tinh th nghim phc tp
-it tn dung mi, ha cht
-t cht thi
-t gy nhim mi trng
PHM VI P DNG
*Thc
phm:
Mi trng
*Cht thi c hi t nh my
* Kim loi nng
*PCB, PAH, dioxins
*Mycotoxins
TRIFLURALIN
TRN NN C
Vortex
13.75 ml AcOH 1%
/ACN
Lc u
6 g MgSO4 v 1,5
g NaOAc
Giai on 2: Clean-up
Ly tm 4000
vng/pht, 5 pht
Chit
lp trn
Lc u, ly tm 4000
vng/pht, 5 pht
Rt 12 ml lp trn, thi
kh bng kh N2
nh mc 1 ml bng
hexane, lc tim vo
my GCMS
1 g MgSO4 + 300
mg C18
Loi mu
C basa
fillet
Ch c
Hi sn
S lng mu
99
11
22
S mu nhim
29
11
10
trifluralin
Hm lng 0,3 n 44,7 1,9 n 158,5 0,3 n 59,1
trifluralin
g/kg
g/kg
g/kg
SPE
QuEChERS
CHIT LNG LNG HAY CHIT RN LNG
LC QUA A
KHC
50 %
37,5 %
31,2%
62,5%
18,2%
Mi thon:
* phn gii tng
* nhy tng, LOD h thp
*o a d lng c hiu qu
HPLC
NEXERA
ACCELA
FLEXAR FX
15
UPLC
AGILENT 1290
L ra hp hn-tp
trung ion vo Q3
L vo rngion vo nhiu
Thc phm
Mi trng
Khoa hc ca s sng
Ch MRM ( ba t cc)
-khc phc: ngoi cht phn tch nhm n, phn no c th nhn din c
thm nhng cht khc bit nu c c s d liu (non-target known
analytes) ci sn trong my (tin ion + 2 mnh ion con + khong thi gian lu
+ t l ion) thng qua phn mm thch hp. S cht nhn din c c th
n vi trm cht.
.
Target:
-cht cn phn tch thng qua GC-MS, LC-MS tt nht l qua
GC-MS/MS hay LC-MS/MS
-i hi c chun v ni chun so snh thm thi gian lu
Non-Target:
-i hi c d liu, ion phn t, ion phn mnh, 2 mnh
ion con, thi gian lu, t l ion
-gii hn bi s d liu trong c s d liu database
Flow rate
Injection volume
Column temperature
: 0.2 mL / min
: 5L
: 40
MS
Nebulizing gas flow
Drying gas pressure
DL temperature
BH temperature
Interface
CID Gas
: SHIMADZU LCMS-8030
: 1.5 L / min
: 10 L / min
: 250
: 400
: ESI
: 230 kPa
B Conc.
B Conc.
B Conc.
B Conc.
B Conc.
B Conc.
B Conc.
Stop
40
60
60
80
100
100
20
Compounds
Methomyl
Methomyl
Acephate
Acephate
Carbendazim
Carbendazim
Isoprocarb
Isoprocarb
Carbaryl
Carbaryl
Fenobucarb
Fenobucarb
Propoxur
Propoxur
Aldicarb
Aldicarb
2,4 D
2,4 D
Carbofurane
Carbofurane
Aldicarb-sulfone
Aldicarb-sulfone
Methiocarb
Methiocarb
Oxamyl
Oxamyl
m/z
CE (V)
163.00>87.90
10
163.00>106.00
12
184.10>124.60
20
184.10>143.00
10
191.90>132.00
31
191.90>160.05
19
194.20>77.00
35
194.20>95.10
16
202.00>127.00
28
202.00>145.10
15
208.10>77.10
30
208.10>95.10
16
210.20>152.90
10
210.20>168.00
10
213.00>70.00
25
213.00>89.00
25
218.85>125.00
30
218.85>161.00
15
222.10>123.10
22
222.10>165.20
12
223.10>123.00
24
223.10>166.20
12
226.10>121.20
12
226.10>168.60
20
237.10>72.10
30
237.10>108.90
30
Compounds
Carbofurane-3OH
Pirimicarb
Pirimicarb
Imidacloprid
Imidacloprid
Thiamethoxam
Thiamethoxam
Tebuconazole
Tebuconazole
Tebuconazole
Flusilazole
Flusilazole
Propiconazole
Propiconazole
Thiodicarb
Thiodicarb
Difenoconazole
Difenoconazole
Chlorantraniliprole
Chlorantraniliprole
Indoxacarb
Indoxacarb
Emamectine benzoate
Emamectine benzoate
Abamectine
Abamectine
m/z
CE (V)
238.50>181.30
10
239.00>72.00
35
239.00>182.00
35
256.00>175.00
15
256.00>209.10
19
291.90>181.00
15
291.90>211.20
25
308.10>57.10
30
308.10>70.00
50
308.10>125.10
40
316.00>165.10
30
316.00>247.15
20
342.00>69.10
20
342.00>158.95
20
355.00>88.10
20
355.00>108.10
20
406.00>187.00
30
406.00>250.95
30
484.00>285.80
15
484.00>453.05
15
528.00>150.00
30
528.00>218.00
30
886.50>81.90
50
886.50>158.25
45
896.00>448.80
45
896.00>751.10
50
CARBENDAZIM
DETECTED
EMAECTIN BENZOATE
DETECTED
DIFENOCONAZOLE
DETECTED
CARBARYL NOT
DETECTED
TEBUCONAZOLE
DETECTED
Compounds
m/z
Re. Time
Area
Result (g/kg)
Compounds
m/z
Re. Time
Area
Result (g/kg)
Methomyl
---
NDCarbofurane-3OH
---
ND
Methomyl
---
NDPirimicarb
---
ND
Acephate
---
NDPirimicarb
---
ND
Acephate
---
NDImidacloprid
256.00>175.00
5.232
5738
ND
4.56
4.563
253980
1378045
5.22 Imidacloprid
5.22 Thiamethoxam
256.00>209.10
5.254
6193
ND
291.90>181.00
4.762
661776
ND
ND
Carbendazim 191.90>132.00
Carbendazim 191.90>160.05
Isoprocarb
---
NDThiamethoxam
---
Isoprocarb
---
ND Tebuconazole
Carbaryl
---
NDTebuconazole
308.10>57.10
308.10>70.00
9.177
9.203
539979
2195189
15.21
15.21
Carbaryl
202.00>145.10
7.925
11669
NDTebuconazole
308.10>125.10
9.203
389237
15.21
Fenobucarb
208.10>77.10
8.59
62695
NDFlusilazole
316.00>165.10
8.997
14170
ND
Fenobucarb
208.10>95.10
8.59
516093
NDFlusilazole
316.00>247.15
9.022
18907
ND
Propoxur
---
ND Propiconazole
342.00>69.10
9.31
254589
4.97
Propoxur
210.20>168.00
7.523
7555
ND Propiconazole
342.00>158.95
9.31
161899
4.97
Aldicarb
213.00>70.00
6.766
16463
NDThiodicarb
---
ND
Aldicarb
213.00>89.00
6.808
5283
NDThiodicarb
355.00>108.10
8.024
24423
ND
2,4 D
---
ND Difenoconazole
406.00>187.00
9.471
4567308
83.58
2,4 D
---
ND Difenoconazole
406.00>250.95
9.48 138018832
83.58
Carbofurane
---
NDChlorantraniliprole
---
ND
Carbofurane
---
NDChlorantraniliprole
---
ND
Aldicarb-sulfone ---
NDIndoxacarb
---
ND
Aldicarb-sulfone ---
NDIndoxacarb
---
ND
886.50>81.90
8.809
326320
6.44
886.50>158.25
8.809
2235497
6.44
10.193
379
ND
ND
Methiocarb
---
Methiocarb
---
Emamectine
ND benzoate
Emamectine
ND benzoate
Oxamyl
---
NDAbamectine
896.00>448.80
Oxamyl
---
NDAbamectine
---
MS
SPIROXAMINE
MS/MS
O
C
N
O
+
m/z = 100,11262
CH3CHO
O
C
O
H H
O
H
m/z = 144,13883
ION PHN T V CC NG V
V. KT LUN
Mt h thng qun l c hiu qu, bt chng cho, d dng qui trch
nhim, hng mnh v xy dng chui thc phm an ton t trang tri
n bn n, cng thm mt h thng labo kim nghim c t chc rt
khoa hc vi trang b hin i chuyn dng v i ng giu kinh nghim,
nng n nhit tnh, c qun l theo mt h thng cht lng c quc
t cng nhn, c m rng thc s theo hng x hi ha, huy ng
c tng lc l cha kha gp phn m bo VSATTP trong nc trong
thc t nui trng v sn xut hin nay.
THNH THT CM N