nhom 9-hptdc

8/13/2019 nhom 9-hptdc

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TrngihcNng Lm TPHCM

Bmn Cng nghha hc

BI BO CO HA PHN TCH DNG C

TIXY DNG QUY TRNH PHN TCH 3MCPD

V CC BC NH GI TRN SN PHM

Gingvin hngdn: Phng V CmHngSinh vin nhm 9 thchin:

1. L ThMng 111390272.ThHuyn 111390663. HunhTNh 111390124. TrnThTNh 111390955. Mai ThVitTrinh 11139177

6. Bi ThPhngDung 11139002


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A. TNG QUAN V 3MCPDI . Tnh chtha hc

I I . Tc hica3MCPDI I I . Giihntiacho php 3MCPD trong ncchmIV.iukinhnh thnh ct

B. MT S PHNG PHP PHN TCH 3MCPDI . GCMS c thlm cg?I I . uv nhcimcaphngphp

C. PHNG PHP PHN TCH 3MCPD THEOGCMS

D. PHNG PHP PHN TCH 3MCPD THEO 52

TCN-TQTP 0010:2005E. NHN XT QU TRNHF. TI LIU THAM KHO


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I . Tnh chtha hc:

3MCPD thucnhm ha chtgy cc tn:chloropropanol (tn khoa hc: 3- monochloropropanne-1,2-diol).

Tntididnghnhpracemic ca2 ngphn (R)

v (S). Cng thccuto:

bnvngca3MCPDphthucvo pH v nhitmi trng.


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I I . Tc hi ca 3MCPD(T liu Cc QLCLVSATTP -B Y T)

Th nghim trn chut cng : Vi 3MCPD 1mg/kg th trng/ngy: tnh trng gim kh nnghot ng vsinh sn chut c

10mg n

20mg/kg:gy tn thng tinh hon,gim kh nngsinh sn chut c Hn 20mg/kg : gy tn thng h thn kinh trung

ng

30mg/kg lm tng trng lng thn ca chutVi 1,3-DCP hm lng ln hn 19mg/kg trng lngtrong nhiu ngy:Gy khi U thn,gan,biu miming,li,tuyn gip v biu ming ung th do bin

i gen .


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III. Gii hn ti a cho php 3MCPD trong

nc chm Chu u (CE 466/2001 ngy 8/3/2001): 0.020

mg/kg cht 3-MCPD c v New Zealand(24/10/2001): 0,2mg/kg

3MCPD + 0,005mg/kg 1,3DCP

Canada(25/11/1999): 1mg/kg cht 3-MCPD i loan: 1mg/kg cht 3-MCPD

Vit Nam(Q 11/2005/Q-BYT) ngy 25/3/2005:1mg/kg cht 3MCPD trong nc tng, x du vdu ho


6/30

IV. iu kin hnh thnh c t:

CH2-O-COR CH2-OH

CH2-O-COR CH-OH + 3 R-COOH

(acid bo)

CH2-O-COR CH2-OH(triglycerid) (glycerin)

CH2-OH CH2-Cl

CH-OH CH-OH

CH2-Cl CH2-Cl

(3MCPD) (1,3DCP)


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* Nghin cuphnnghnh thnh v phn hy3MCPD(DOLEZALM, CALTAP, VELISER) thyrng:

Glycerol + Cl- k1 Cloropropanol

k2 Phn hy

* Cngphnngto3MCPDphthucmnhvo nhit . iukintiul 2300C th lng3MCPD tothnh l 50mg/kg glycerol tham giaphnng. 1000C th lng3MCPD tothnh chl

0.6mg/kg.

* Hngstcphnngto3MCPD k1 tglycerol nhhnhngstcphnngphn hy

3MCPD k2 (k1


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Sck lngcao

p

Sck kh ghpkhiph


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S cu to u d khi ph Cu to u d khi ph by ion
http://www.google.com.vn/url?sa=i&rct=j&q=quy+tr%C3%ACnh+ph%C3%A2n+t%C3%ADch+3mcpd+theo+ph%C6%B0%C6%A1ng+ph%C3%A1p+GC-MS&source=images&cd=&cad=rja&docid=zpq9jL3kQK2PXM&tbnid=DNjlL9i6LV8dEM:&ved=0CAUQjRw&url=http://www.case.vn/vi-VN/87/88/141/details.case&ei=dB5VUe-3DIfBrAf4tYCoCQ&bvm=bv.44442042,d.bmk&psig=AFQjCNEgL7XB-b449v-Z6DVe8wTRZXBFsA&ust=1364619035691710http://www.google.com.vn/url?sa=i&rct=j&q=quy+tr%C3%ACnh+ph%C3%A2n+t%C3%ADch+3mcpd+theo+ph%C6%B0%C6%A1ng+ph%C3%A1p+GC-MS&source=images&cd=&cad=rja&docid=zpq9jL3kQK2PXM&tbnid=DNjlL9i6LV8dEM:&ved=&url=http://www.case.vn/vi-VN/87/88/141/details.case&ei=mx1VUcORDs3HrQfCjYHABQ&bvm=bv.44442042,d.bmk&psig=AFQjCNEgL7XB-b449v-Z6DVe8wTRZXBFsA&ust=1364619035691710


10/30

Phngphp Sck kh kthpviKhiph,phngphp mnhmvinhycao

BnchtGC-MS: skthpcaSck kh (GasChromatography) v Khiph(Mass Spectometry)Ngngpht hinphngphp ny:1 picogram.

I. GC-MS c thlm cg?

Phn tch: GC-MS c thphn tch cc hnhphachtphctptrong khng kh hay trong nc, tccquytnhbitnh bay hi.

nhlng: GC-MS c thnhlngmtchtbng

cch so snh vimuchun, l chtbittrcv cnhlngchunbngGC- MS. Nhndng:Nutrong muc mtchtlxuthin, khi

phnhndngcutrc ha hccnht, sau so snh

vimtthvincutrc cacc chtbit.


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Phn tch hn

hpha cht.Phnsc

k kh (GC)

nhtnh. nhlng.Phnkhiph(MS)

GCMS GM 2 THNH PHN


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Squy trnh phn tch

Kimnhnctng
http://www.google.com.vn/url?sa=i&rct=j&q=quy+tr%C3%ACnh+ph%C3%A2n+t%C3%ADch+3mcpd+theo+ph%C6%B0%C6%A1ng+ph%C3%A1p+GC-MS&source=images&cd=&cad=rja&docid=RzgBczGhK11dtM&tbnid=l5UbRnD5oxheMM:&ved=0CAUQjRw&url=http://dantri.com.vn/event/nuoc-tuong-co-chat-ung-thu-942.htm&ei=MjRVUcDjIcv-rAe1wICYAQ&bvm=bv.44442042,d.bmk&psig=AFQjCNEU4S1diyLL34hXf-UFT6ZlA27aFw&ust=1364624766219950


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II. uvnhcimcaphngphp

uim

Tnhbay hi

Nhit

Thi

gianqutnhanh

nhycao

Nhcim

Phiiuchdn

xut

p sut

Loictsck

Githnhcao


14/30

Phm vi p dng: xc nhhm lng3-monoclo propan1,2-diol (3MCPD) trong x du, nctngv duho

Nguyn l:* Muccho hpphqua ctextrelut, giihp3-MCPD

bngdietyl te.* Tipcho todnxutvidung dchacid toluen-4-

sulfonic trong aceton thnh 4-(clometyl)-2,2-dimetyl-1,3-

dioxolan, (T=40C, 90).

* Sau cng otrn my sck kh videtector khiph(GC/MS).

Gii hn pht hin ca phng php: 4,01 ppb.Gii hn nh lng: 13,37 ppb.


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Dngc:* Cn phn tch (chnh xc nmg)* Bnh nhmc100ml, 50ml, 20ml, 10ml* Bnh cuct250mlQ* Ccthytinh 10ml, 50ml, 100ml* Pipet 1ml, 2ml, 3ml, 4ml, 5ml

* ngthytinh c npvn5ml, 10ml* Xylanh, athytinh* Phulc, giylc

Thitb:* Bctquay chn khng* Hthngmy sck kh

khiph


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Yu cuivi hthngsck kh khiph:

C thsdnghthngTrace GC-Trace MS Plus(Hng snxutThermo Finigan) hoccc hthngmysck kh khiphtngngvicuhnh kthuttithiu:

+ u d khi ph+ B phn tim mu chia/ khng chia dng(Split/Splitless Injector), chng trnh nhit (PTVInjector: Programmed Temperature Vaporation Injector)

+ Ct sc k mao qun SPB 1701, di 30m,ng knh 0.25mm, lp film 0.25m.+ My tnh iu khin thit b v x l d liu.


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iukinchymy*iu kin sc k:

- Chng trnh nhit ct :+ Nhit u 45oC, gi 1 pht;+ Sau tng ln 120oC vi tc gia nhit

6oC/ pht;+ Tip tc tng nhit n 250oC, tc

gia nhit 15oC/pht, gi nhit ny 5pht.- Tim mu vich khng chia dng

+ Nhit b phn tim mu : 250oC+ Th tch mu tim : 2l

Tc kh mang He : 1,5 ml/pht


18/30

*iu kin khi ph:- MS Tune file:

+Ngun Ion ha : EI+Nng lng ion ha : 70eV+Nhit ngun ion : 180oC+Nhit Interface: 200oC

+ Gi tr ca b khuch i Multiplier : 300 500V- MS method

+ Chqut Fullscan:

- Thigian qut : 5 - 15 pht- Khongkhiqut : 35 - 150 amu+ Chqut Ion chnlcSIM

- Skhilachnqut: 135- Thigian qut : 610 pht


19/30

Ha cht, thucth: ha chtsdngc tinhkhitphn tch (TKPT), dung mi l dung mi dng

cho sck.* Chtchun3-MCPD* Diethyl ete loidng cho sck* Aceton loidng cho sck

* Acid toluen -4-Sulfonic* Ethyl acetat loidng cho sck* CtExtrelut: Dng xylanh 60ml, nhibng thy

tinh vo ungxylanh. Sau cho t t 10g ht

Extrelut vo xy lanh, dng athytinh g nhvothnh ngcho htxunguv cht.* Natri clorua: Dung dchbo ho trong nc* KhNit99,999%

* Kh Hli 99,999%


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Pha chdung dch

*Dung dchacid toluen-4-sulfonic trong Aceton(1g/L): Cn chnh xc 0,1000g acid toluen - 4 -sulfonic cho vo bnh nhmc100ml, nhmc

nvchbngaceton, lcu.

*Dung dchchun3-MCPD 100ppm: Cnchnh xc 0,0100g 3-MCPD cho vo bnh nhmc100ml, nhmcnvchbngethyl acetat, lcu.


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*Dung dchchun3-MCPD 10ppm: Ht 1mldung dch3-MCPD 100ppm vo bnh nhmc

10ml. nhmcnvchbngethyl acetat, lcu.

*Dung dchchun3-MCPD 200ppb: Ht 1ml

dung dch3-MCPD 10ppm vo bnh nhmc50ml. nhmcnvchbngethyl acetat, lcu.

*Dung dchchun3-MCPD 20ppb: Ht 2mldung dch3-MCPD 200ppb vo bnh nhmc20ml. nhmcnvchbngethyl acetat, lcu.


22/30

Chunbmu:

* Cn 4g mu, chnh xc n0,001g vo ccthytinh 50ml. Thm vo 8g dung dchNaCl boha, khuyu.

* Cho ton b dung dch trn vo ct extrelut. n nh 15 pht cho ton b nc v chttrong dung dch phn b u trn b mt ca htextrelut.

* Ra gii 3-MCPD bng 150ml dietyl te, thudch vo bnh cu ct. Sau em c quay chnkhng n gn cn, ri dng kh nit thi kh.


23/30

Dn xut ha:

* Dng pipet ht chnh xc 2ml dung dchacid Toluen-4-sulfonic trong aceton (1g/L) vo

bnh cu ct

* Lc u ri chuyn ton b dung dch nyvo ng nghim c nt. t ng nghim vo

bp cch thy 40oC trong 90pht

* Ly ra ngui nhit phng, sau chuyn vo chai 1,5ml o trn my GC/MS(dch th).


24/30

ng 1 ng 2 ng 3 ng4

3-MCPD chun(20ppb) chovo ctextrelut

1ml 2ml 4ml 6ml

Dung dchsau ragiibngdietyl te

C quay chn khng n gn cn,thi kh bng kh Nit

Dung dchacid Toluen-4-Sulfonic trong aceton (1g/L) 2 ml

Lc u, t cc ng nghim vo bp

cch thy 40oC trong 90 pht. ngui nhit phng, chuyn

vo l 1,5ml o trn my GC/MS

Nng 3-MCPD chun (ppb) 10 20 40 60

Chunbmuchun:


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Xy dng ng chun:* Kim tra thit b c chy n nh theo cc

iu kin m t

* Ln lt tim cc mu chun c chun b.* Ghi li din tch pic tng ng vi tng nng .* Thit lp phng trnh biu din tng quan tuyn

tnh gia nng chun v din tch pic.

Tinhnh phn tch :

* Tinhnh tim muphn tch vo my, ghi lisckmilntim mu.

* Ghi lidintch c thigian luvphkhitngngvithgian luvphkhicachtchun.

* Davophngtrnhbiudintngquan tuyntnh gianngchunv dintch pic, tnh nng

3-MCPD c trong dchth.


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SCKVPHKHICACHUN3-MCPD


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Tnh ktqu:

* Hm lng3-MCPD trong muthctnhtheo cng thcsau :

Cx * V

C (ppm) = Fm

* Trong :- Cx: nng3-MCPD trong dchth(ppm).

- m: khilng muemphn tch (g).- V: thtch cui(ml).- F: hspha long khi o(F=1: khng pha

long)


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Sck kh ghp khiph(GC/MS) l mttrong

nhngphngphp sck hininhthinnayvinhyv chiucao v csdngtrong cc nguyn cu v phn tch kthp.

Hiusutthu hitnhbng% (X) theo cng thc:

Trong :

XR: Lnghotchttm thytrong mutrngcho thm hotcht.

Xo: Lnghotchttm thytrong mutrng.XA: Lnghotchtavo mutrng.

X : % Thu hi.


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Diendancongnghehoahoc.vnbb.com

Ykhoanet.com/NCKH/bsnguyendinhnguyen/3-

MCPD.htm

Forum.vietpet .com

http:/ /vi .wikipedia.vn

ht tp ://tai-l ieu.com /tai-l ieu/tong -quan-ve-3-

mcpd-888/


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