DAI HOC QUOC GIA HA NOI
TRITONG
DAI HOC KHOA HOC
T\S
NHIEN
Khao sat va phat trien quy
trinh
phan
tich
cac doc
td
huu ca kho phan huy thuoc nhom
ankylphenol va bisphenol A trong
nu6c
rac
tai mot sd khu vuc bai rac Ha Noi.
MA SO: QT-04-34
CHU TRI DE TAI: GS.TS. Pham
Hiing
Viet
CAC CAN BO THAM GIA:
ThS.
Tran Thi
Liau
HVCH. Tran Thi Tuyet Mai
HVCH.Trinh Thi Thdm
CN. Le Thi Ngoc Ha
OAI HOC QUOC GlA
h-
.v'C
TRUNG TAM THONG TIN

HVCH. Tran
Thi
Tuyet Mai
HVCH. Trinh Thi Tham
CN. Le Thi Ngoc Ha
4.
Muc tieu va noi dung nghien
cufu
Miic
tieu
ciia
de tdi:
- Nghien cuu khao sat va hoan thien quy trinh xac dinh cac hoa chat huu ca
tich
luy
b6n
thuoc
hg
ankylphenol
(4-nonylphenol,
4-t-octylphenol,
4-n-octylphenol)
va
bisphenol A trong cac
mSu
nuac rac.
- Ung dung quy trinh khao sat vao viec phan tich cac din xuat phenol nghien cuu trong
m^u
nuac rac va nuac ngam thuc te
dugc

tich
va xac dinh cac hgp chat nghien cuu trong cac miu thu thap.
- Xu ly, tdng ket cac ket qua phan tfch va viet bao cao.
5. Tom tdt ket qua nghien
cuii
dat duoc
- Da khao sat va hoan thien quy trinh xac dinh cac ankylphenol va bisphenol A trong
miu
nude
rac vai viec ap dung ky thuat chiet pha rin SPE (chat hap phu
CIS),
ket hgp
vdi ky thuat din xuat axetyl hoa vdi dp lap lai cao. Hieu suat thu hdi cua cac hgp chat
nghien cuu deu
>84%.
- Ket qua ap dung quy trinh khao sat thu dugc de xac dinh cac hgp chat 4-nonylphenol,
4-tert-octylphenol,
4-n-octylphenol, bisphenol A trong cac miu nuac ngam va
nude
rac
tai hai khu vuc bai rac lan
ciia
Ha Npi la Nam San va Tay
M6
cho thay su cd mat cua
cac hgp chat nay trong cac miu phan
tich.
Ham lugng trong cac miu
nude
rac nim

6.2. Giai trinh cac khoan chi:
- Thue khoan chuyen mon:
- Quan ly phf:
- Dien
nude
va xay dung ca sd vat chat:
- Hd trg dao lao va NCKH:
- Hoa chat,
nguyen
lieu, dung cu:
9.720.000d6ng
720.
000 ddng
720.000 ddng
540.000 ddng
6.300.000 ddng
KHOA QUAN LY
CHU NHIEM DE TAI
GS.TS.
^4^y^^^
Mi^
^/
GS.TS.
Pham
Huna Viet
TRUONG DAI HOC KHOA HOC TU NHIEN
#H6
HI^U
TRUONG
BRIEF OF THE PROJECT

bisphenol A in leachates samples with significant reliability on spiked samples.
- Carry out collecting leachates samples, groundwater and surface samples around
some landfills in Hanoi (Namson, Taymo dumping sites).
- Analysis and determination target compounds in taken samples,
- Calculation, summarization the obtained results and writing the report.
5.
Actives and Results obtained
- Investigated and developed for analytical procedure of alkylphenols and bisphenol A
in leachates samples with application solid phase extraction (SPE) technique using
C18
cartridge and dramatization technique using anhidrite acetic derivative. The values of
recoveries for every target compounds achieved over 849c and high repeatability.
- The results of application researched procedure to
detennine
4-nonylphenol.
4-terl-
octylphenol, 4-n-octylphenol and bisphenol A in leachates and groundwater samples at
locations of selected dumping sites shown the presence of these compounds in
analyzed samples. Concentrations of nonylphenol and bisphenol A in leachates
samples were ranged 447,5- 1856,3 ng/L and 767,9-7250,1 ng/L, respectively.
Concentration of nonylphenol in leachates samples at Namson dumping site exceeded
United States and Europe standard regarding the predicted no-effect concentration in
water
(PNECy,a,er)
although leachates treated.
- The results contributed assessment and monitoring spatial distribution and behavior
of alkyl phenols and biphenyl A in the environment. The measured data indicated
potential risks of target compounds for wildlife and human health. Further research
need to be continued in the future to get an overview about these compound in the
environment.

thieu ve
MP 5
2.2.2. Giai
thieu ve
OP 5
2.23.
Ung dung
cita
AP 6
2.2.4.
Nguon
thdi AP vdo moi trudng 6
2.2.5. Tdc dgng
ciia
cdc AP ddi vdi dgng thuc
vgt
vd con nguai 7
2.3.
Nude
rac va cac van de nay sinh trong cac bai chon lap rac d Viet Nam
^
2.4. Phuang phap tach chiet pha rin vdi viec tach chiet cac hgp chat AP va
9
BPA
2.5.
Ky thuat din xuat hda
11
IIL
THUC NGHIEM 11
3.1.

I4
IV: KET QUA
VA
THAO LUAN
15
4.1.
Ket qua qua trinh din xuat hda
I5
4.2.
Xac dinh phan manh dac trung ciia cau ttr can phan
tich I5
4.3.
Khao sat quy trinh phan tfch
jy
4.4.
Khao sat hieu suat thu hdi
ciia
quy trinh phan tfch cac dan xuat phenol
\^
trong miu
nude
rac
4.5.
K6't
qua phan
tich
miu
nude
rac thuc te 19
4.5.1.

rtra
giai 17
Bang 6: Kd't qua hieu suat thu hoi ciia cac hgp chat phan tfch trong miu 19
nude
rac tai ndng do
50ng/L
Bang 7 : Ket qua phan tfch miu nude tai bai rac Tay Md 20
Bang 8: Ham lugng cac hgp chat phan tfch trong cac miu tai bai rac Nam
21
San
DANH SACH CAC HINH
Trang
Hinh
I.
Cong thuc phan tu cua BPA 2
Hinh 2: Cong thuc
c^'u
tao ciia nonylphenol 5
Hinh 3: Cong thuc
c^'u
tao ciia OP va NP 6
Hinh 4: Cau
true
ciia hocmon nu tu nhien 17P-estradiol va hoocmon nu 7
nhan tao 4-nonylphenol (mpt dang ddng phan).
Hinh 5: Cac budc tien hanh cua phuang phap chiet pha rin 10
Hinh 6: Ca che phan ung din xuat axetyl hda cacphenol
16
Hinh 7: Dd thi bieu diSn ham lugng NP va BPA trong cac mau
nude

de'n he thdng sinh san, tap
tinh
sinh hoat, tao ra cac u ac
tinh
va gay hau qua nghiem
trpng cho cac the he tuang lai ma khd cd thi du bao trudc dugc. Trong dd, cac din xuat
phenol nhu ankylphenol va bisphenol A ndi trpi len do
tijf
lau da dugc ung dung rpng
rai trong cac hoat dpng sdng ciia con ngudi.
Ankylphenol
(APs),
san
ph^m
thoai bien
ciia
ankylphenoletoxilat, la loai hgp
chat dugc dung pho bien trong cac nganh cong nghiep, sinh hoat va cac ung dung
thuang mai (cong nghiep giay, vai sgi, san,
nhua,
san xuat chat tay
rii"a
sinh hoat va
cong nghiep); bisphenol A (BPA) dugc
diing
lam chat trung gian trong san xuat nhua
policaebonat va chat cham chay, chat ket
dinh,
chat bao phii bao ve, san, vat lieu xay
dung, giay nhiet, vat lieu bao ve dd dien, dien

rac la rat khd khan.
Nghien cuu nay dugc thuc hien vdi muc dfch khao sat va hoan thien quy trinh
xac dinh cac hgp chat ankylphenol va bisphenol A trong miu
nude
rac
sir
dung ky
thuat chiet pha rin ket hgp vdi ky thuat din xuat axetyl hoa. Ben canh dd de gdp phan
vao viec theo ddi, danh gia su phan bd, du doan nguy ca 6 nhilm
ciia
cac hgp chat nay
trong moi trudng, chiing toi da ap dung quy trinh nghien cuu de phan tfch mot sd miu
nude
rac va
nude
ngam thu thap tai hai bai rac Nam San va Tay
M6.
H.
TONG QUAN
2.1.
Gidi thieu ve Bisphenol A (BPA)
Bisphenol A (BPA) la ten thong dung cua 2,2-(4,4-dihidroxydiphenyl)propan.
Cong thuc
ciia
BPA thu dugc bing each ket hgp 2
moi
phenol vdi 1
moi
axeton nhu
mieu ta dudi day:

l,195g/cm3
220^C(d4mmHg)
398"C(d760mmHg)
150-155"C
9,59—10,2
120
—300mg/l
2.1.2. Ung dung
ciia
BPA
Gin nhu toan bp (99,9%) san pham ciia BPA dugc
sir
dung nhu mot chat trung
gian ciia qua trinh san xuat nhua polycacbonat, chat deo tong hgp epoxy, chat lam
cham chay hay mpt sd san phim chuyen dung khac. BPA cdn cd mat trong nhung san
pham nhu chat dfnh, chat
Idt
phu, bpt san, vat lieu xay dung,
dia
compact, vat lieu
quang hpc, giay chiu nhiet, bao gdi. Ngoai ra nd cdn dugc six dung trong cong nghiep
nhupm hoac san xuat vd nhua ciia cac thiet bi dien. BPA ciing dugc diing la chat uc che
phan ung hoac chat chdng oxi hoa trong qua
trinh
san xuat PVC.
2.13.
Nguon thdi BPA vdo moi tru&ng
Ngudn thai BPA
chii
yeu la

2J.4.
Tdc
dpng ciia
BPA ddi voi dong thuc vgt vd con ngudi
BPA la mpt trong nhiing hoa chat tong hgp kha
bin
trong moi trudng. Mot vai
nghien
ciiu
vl dpc tfnh cua BPA ddi vdi cac loai vi sinh vat, tao, dpng vat khong xuang
sdng, ca va con ngudi da chiing minh nd la mpt chat cd tilm nang gay
6
nhiem moi
trudng nghiem trpng, de doa he sinh thai. Tieu chuan ciia My va Lien minh chau Au vl
ndng dp cua BPA trong moi trudng nude la 1000
ng/1.
Bdng 2: Dgc tinh
ciia
BPA ddi vdi mot sd dgng thuc vgt thuy sinh
Loai
Vi sinh vat
nude
ngot
Pseudomonas putida
Pseudomonas flourcscens
Bp chet nude Daphnia
magna
Tom cam Mysidopsvbahia
Ca tue dau to Pimephales
promcias

vong
Tu vong
Gia tri
(mg/l)
>320
54,5
3,9
M
4,6
3-3,5
15
9,4
7,5
Tham
khao
17]
|13|
[13]
151
[51
[8]
[9]
[13]
[12]
Nhung anh hudng chu yeu
ciia
BPA la len he thdng npi tiet nhu kfch thfch hay
kim ham hoat dpng cua hoocmon gidi tfnh ddi vdi dpng vat, cd the din den nhung hau
qua nhu: +)anh hudng den
sir

non),
anh hudng den viec tao tinh triing cung nhu su phat trien cua ca
thi.
d nhirng ca the
nay ngudi ta da tim thay nhung te bao budng triing trong tinh hoan. Mpt vf du khac, tai
Nhat Ban, khi nghien
ciiu
eac loai ca sdng trong moi trudng nude ed chiia BPA (tai
ndng dp 1820
|^g/l)
da phat hien nhilu ca
thi vira
cd budng triing
vira
cd tinh hoan.
Nhu vay tai ndng dp nay, xu hudng bien ddi gidng la lam tang gidng cai. Dilu nay cd
anh hudng
Idn
den sd lugng ciia loai.
Nhung dpng vat thiiy sinh khong xuang sdng
cijng
td ra nhay cam vdi BPA.
Dpng vat than
mIm
phan
iing
vdi chat nay d ndng dp rat thap. Thf nghiem tren loai
ihfm mIm
Potamopyrgus
antipodanmi

Cac AP dudi dang ankylphenol etoxylat (APE) la nhdm cac chat hoat dpng bl
mat dugc phd bien nhat hien nay. Trong dd khoang 80% la cac nonylphenol etoxylat
(NPEs). Cac
octylphenol
etoxylat (OPEs) cung dugc su dung nhu mpt chat hoat dong
bl mat khong phan ly trong cac thudc trii sau vdi mot lugng nhd trong tdng san luang
tieu thu.
Trong 40 nam gan day, 450 trieu tan nonylphenol (NP) dugc san xual tren loan
the gidi, chi rieng tai Hoa Ky, con sd nay la 150 000 tan. Day la mpl hoa chat long
hgp rat dpc hai. Nd cd kha nang tfch tu sinh hpc, trong cac mo
ciia
ca
thi
sdng va
ifch
tu trong mdi trudng. NP da dugc xac dinh trong cac miu moi trudng d My, Canada va
(Thau Au, dan tdi nguy ca gay 6 nhiem tai cac hd va cac ddng song.
22J,
Gi&i thieu veNP
NP bao gdm nhieu ddng phan vdi chudi
nonyl lien
ken
true
tie'p vdi vdng tham
cua phan tit phenol. 4-NP, cha't cd gdc nonyl nim d vi trf ddi dien vdi nhdm hidroxy la
hgp chat phd bien nhat, chie'm khoang 90% NP thuang mai.
HO
X ^C,H,3
Hinh 2: Cong thuc cdu tgo cua nonylphenol
4-NP la chat long, sanh, cd mau vang nhat, trong sudt, cd mui phenol nhe. Cac

la 5,34 mg/l), tan tdt trong
benzen, anilin, heptan, etylenglycol.
NP cd tfnh
ua
ma nen nd cd kha nang tfch tu trong cac mo ma hay trong ca the
ciia
cac dpng vat.
2.2.2. Gioi thieu ve OP
Cong thiic phd bien nhat
ciia
4-OP la
para-tertoctylphenol
hay 4-(l,l,3,3-
tetrametylbutyOphenol
OH OH
n - octylphenol tert - octylphenol
Hinh 3: Cong
thitc
cdu tgo cua OP vd NP
4-OP tdn tai d dang tinh
thi
tring hoac bui vdi mot sd hing sd vat ly sau
Cong thiic phan tir:
C14H22O
Nhiet dp ndng ehay:
81-84°C,
nhiet dp soi:
150°C
(d 4 mmHg). Ty trpng 0,961
g/cm\

xuat nhua PVC. AP ciing dugc dung nhu chat phu gia trong dau ma boi tran
Nonyl- va octylphenol la nhiing sin phim
bin ciia
qua trinh phan huy sinh hpc
cac APE, chiing dugc san xuat khoang 10 000-50 000 tan/nam trong dd udc tfnh san
lugng
ciia
toan chau Au la 6800 tan.
2.2.4. Nguon
thdiAP
vdo moi tru&ng
Hiu het
Ctic
AP dugc thai ra moi trudng dudi dang APEO, chat nay tiep tuc
thoai bien thanh ankylphenol mono hay dietoxylat rdi hap thu trong
biin
va tram tfch.
Ahel
va cpng su (1994) da udc tfnh trong mpt chu trinh xir ly
nude
thai khoang 40%
NP dugc xir ly, 20% hap thu vao
biin,
cdn lai 40-45% khong
xii
ly dugc va di vao cac
ddng chay.
Ngudn thai chfnh
ciia
AP vao moi trudng la tir cac sin pham tay rira, mpt sd san

ciiu
tren toan the gidi da dua
ra nhirng canh bao vl tinh trang
6
nhilm moi trudng, va nhiing tac dpng cd hai gay ra
bdi cac hoa chat lam rdi loan tuyen npi tiet. Mpt vai nha khoa hpc da chiing minh rang
nhirng hgp chat nay cd anh hudng den he sinh san,
tap
tfnh hoat dpng
ciia
con ngudi
cung nhu cac loai khac, gay ra nhirng u ac tfnh va nhiing hau qua nghiem trpng khac
cho the he tuang lai.
Dpc tfnh
ciia
APs tang theo chilu dai
ciia
chuoi ky nude va dugc
thi
hien khi
chiing phan bd vao cac mang ma eua ca the nhu mang cua bp may gongi gay gian
doan viec tdng hgp ra nang lugng. Nhirng tac dpng
ciia
AP bit dau d ndng dp khoang
l,5mg/l.
Tuy nhien NP the hien tfnh dpc d ndng dp thap han nhieu, khoang
0,112
mg/l
ddi vdi ran nude. Nhin chung cac AP dpc han APEO, vf du NP dpc han NPEO khoang
10 lin.

dao cua
chudt
gidng nhu hien tugng dien ra vao chu ky dpng
due,
Su sirng hda ciing
xay ra khi thir
nghifm
vdi
4-tert-pentylphenol
nhung khong xay ra vdi 2-n-
pentylphenol. Dilu nay dugc giai thfch do su khac nhau
ciia
2 nhdm the d vdng
benzen.
Bang chiing tie'p theo dugc cong bd vao nam 1978 khi Mueller va Kim nghien
ciiu
thay rat nhilu AP cd
thi
thay the cac estradiol lien ket vdi ca quan thu nhan.
Nhung tac dpng nay xay ra manh tai nhiet dp thap
(0-4^^).
Tuy nhien, nhiing ket qua nghien cuu tren khong
gay
dugc su quan tam rpng rai
cho
6€n
nam 1991, khi Soto va cac cdng su tinh cd phat hien 4-NP trong khi thf
nghiem
tr6n
cac te bao ung thu vu MCF7, nhay cam vdi estrogen. Hp phat hien thay

6
Viet Nam
[4,51
Nude
rac cd
thi
dinh nghia nhu mpt chat
Idng
tham qua chat thai rin, mang theo
cac chat hoa tan va chat rin la
lirng.
Trong phan
Idn
trudng hgp, nude rac dugc sinh ra
do qua trinh xam nhap
ciia
cac ngudn nude tir ben ngoai vao nhu he thdng thoat
nude
bl mat,
nude
mua,
nude
ngim va nude dugc sinh ra do qua trinh phan huy chat thai
trong bai chon lap .
Lugng nude rac hinh thanh trong cac bai chon lap dugc udc tfnh dua tren su can
bing nude trong bai chon lap.
Sir can
bing
nude
bao gdm tong lugng nude di vao bai

hoi thdi bdc len do qua trinh
phan huy yem khf trong bai rac. Vi vay, da gay ra
6
nhilm khong khf va ngudn
nude
ngam ca mpt viing rpng
Idn.
Cac bai chdn
la'p
rac d thanh phd
Idn diu
trong tinh trang qua tai, khong dugc
thid't
ke va quy hoach ngay tir dau, cpng vdi vice quan ly van hanh yeu kem nen da gay
ra hang loat cac van dl het
siic
nan giai.
Nude
rac sinh ra tir cac bai chon la'p (chu yeu la tir cac hd tfch trir
nude
rac bd trf
xung quanh bai rac) chay tran ra ngoai he thdng bd bao
gay
thiet hai nang nl cho ddi
sdng san xuat va sinh hoat cua dan cu. Nude rac sinh ra khong dugc xir ly kip thdi
hoac chua dat tieu chuin dang ed nguy ca
gay 6
nhiem nude ngam va viing nong
nghiep xung quanh.
Viec giam thieu va phan loai chat thai rin tai ngudn hau nhu chua dugc quan

khac nhau. Chat long dugc dua qua cot dudi tac dung
ciia
ap suat hoac chan
khong.
w
2.
DDC
M
3.
^A^
fi
A
u
Rira giai
cac chat anh hudng
fi
A
w
chat phan tfch
Hinh 5: Cdc budc tien hdnh
ciia
phuang phdp chiet pha rdn
Phuang phap chiet pha rin gdm 4 budc, dugc mo ta nhu hinh 5.
Budc 1: Vat lieu nhdi cot dugc lam udt va solvat hda cac nhdm chiic. Budc nay
cdn cd nhiem vu loai bd khdng khf d cac khoang trdng giira cac hat vat lieu hap phu.
Budc 2: Dung dich miu dugc chay qua cot. Chat phan tfch va mot vai thanh
phin anh hudng dugc
giir
lai, cac thanh phan khac khong bi hap phu dugc loai ra ngoai.
Budc 3: Loai bd cac chat anh hudng ra khdi cot, chi giii lai chat phan tfch. Cd

d^n
xuat hda
Viec phan tfch cac AP va BPA bing phuang phap sic ky thudng gap khd khan.
Pic thu dugc thudng thap, nhilu va khd nhan dang do cd nhdm OH phan cue cd kha
nang luu giir lau vdi pha
tinh
cua
c6t
sic ky
gay
ra hien tugng keo chan pic, can trd
viec dinh tfnh, dinh lugng mpt each chfnh xac.
Dc khac phuc hien tugng tren ngudi ta thudng sir dung ky thuat din xuat hda,
thay the nhdm OH phan cue bing cac nhdm chiic khac ft phan
cue
han. Cac ky thuat
thudng diing dl dan xuat hda hgp chat phenol la
silyl
hda, axetyl hda, metyl hda
Trong nghien
ciiu
nay, chiing toi lua chpn phuang phap axetyl hda cac phenol
bing anhydrit axetic. Phan
iing
nay dien ra nhanh, dinh lugng tai nhiet dp phdng. Phan
ling dugc mo ta nhu sau:
OH OOCH
C
H X O O N
a ,, ,

hang Merck dugc sir
dung lam tac nhan axit hoa va din xuat hoa.
Cac dung moi diclometan, hexan, axeton va metanol loai tinh khiet phan tfch
cua Merck.
Nude cat 2 lin dugc lpc qua thie't bi khir ion hoa Millipore (Nhat Ban).
Cha't ha'p phu florisil (90-100 mesh) sieu tinh khiet
ciia
Supelco va
Na2S04
khan
dang tinh khiet phan tfch
ciia
Merck dugc nung trong
Id
qua dem tai
450*'C.
Sir dung
c6t
chiet pha ran vdi cha't hap phu
RP-18
500mg cua hang Merck.
3.2.
Thiet bj
can
phan tfch Metier cd dd chfnh xac
lO'^g.
Til say,
tii
hot, bp cat duoi dung moi bing khf
N2

phan huy
ciia
cac vi sinh vat va dugc bao quan tai 40C cho den khi chiet phan tfch.
33.2 Khao sdt giai dogn lam sach tren cgtflorisil
3.3.2.1.
Chuan bi cot nhoi
Cot lam sach tu nhdi florisil dugc chuin bi nhu sau: Chuan bi cot sic ky thuy
tinh dai 50cm, dudng kfnh trong 1cm da dugc lam sach, say kho. Can chfnh xac 5g
chat hap phu florisil da dugc say trong
Id
nung qua dem tai
200^C
vao trong cdc thuy
tinh nhd. Them dung moi n-hexan den ngap bl mat florisil. Qua trinh nhdi cot udt
dugc tie'n hanh lan lugt nhu sau; cot dugc nhdi dau tien la ldp bong thuy tinh, tiep den
la ldp
Na2S04
khan rdi 5g florisil. Tren ciing la 1 ldp
Na^SOj
khan. Go nhe phfa thanh
ngoai cot dl chat hap phu dugc nen chat.
Chii
y trong khi nhdi cot khong dugc de cot
kho.
3.3.2.2. Khao sdt luang dung moi nh gidi
- Them
true
tiep 10
jil
surrogate BPA- dl4 ndng dp 10 mg/l, 2

ml axeton va chuyen sang dng nghiem cd vach. Tiep tuc co dung moi bing ddng khf
nita vl 0,5 ml. Axetyl hda hdn hgp bing anhidrit axetic. Them
\0\i\
npi chuin
naphtalen- d8 10 mg/l, dinh
miic
vl 1ml. Lie manh trong vai giay bing thie't bi lie rdi
tien hanh bam len GC/MS dl phan tfch tu dpng theo chuang trinh dat sin.
3.3.3. Khao sdt hieu sudt thu hoi cua phuang phdp
Quy trinh kilm tra hieu suat thu hdi dugc tien hanh nhu sau;
- Chuan bi miu them chuan bing
each
lay 10 ml miu nude rac them vao dd 100
jil hdn hgp chuan 500
|ag/l,
10 |il BPA- dl4 10 mg/l rdi thuc hien quy trinh phan tfch
nhu tren.
- Lam them miu tring bing
each
lay 10 ml nude ca't 2 lan, them vao 10
\JL\
BPA-
dl4
10 mg/l va tien hanh theo quy trinh phan tfch d tren
3.4.
Phan
tich
dinh tinh va dinh luong tren GC/MS
+j
Pha dung dich chuan:

Trong dd:
CS la ndng dd cua cha't cin phan tfch trong miu.
a la dp ddc
ciia
dudng chuin.
b la doan chin cua dudng chuan.
AS la
di6n
tfch cua cha't
chu^n
phan tfch do dugc tren GC/MS.
AIS
la dien tfch cua chat npi chuan do dugc tren GC/MS.
IIS la lugng chat npi chuan dugc them vao miu.
S la lugng miu phan tfch ban dau.
+j
Dieu kien lam viec
ciia
thiet bi GC/MS:
Cac hgp chat nghien
ciiu
dugc phan tach bang viec sir dung thiet bi sac kf khf
GC/MS-
QP2010
cua hang Shimadzu nhirng thong sd sau:
-
Cot mao quan DB-1 (dp dai cot la 30m, dudng kfnh trong 0,32mm, dp day ldp pha
tinh
0,25^m).
- Khf mang He (dp tinh khiet 99,999%) dugc sir dung la khf mang vdi tdc dp 2ml/phiit.

Dich lpc
ciia
miu dugc chiet bdi ky thuat chiet pha rin vdi cot SPE
RP-18,
da
dugc rira lin lugt ciing vdi 20ml n-hexan, 20ml DCM, 20ml MeOH va 10ml
nude
cat
khir ion. Cho 200ml dich lpc miu di qua cot SPE vdi tdc dp
lOml/phiit.
Cac chat can
tach chiet dugc rira giai ra vdi 20ml MeOH.
Dua them
10)^1
chat surrogate
BPA-dl4
vao dich rira giai dugc de lam chat ddng
hanh, tfnh gia tri hieu suat thu hdi.
Dich rira giai dugc co cat quay chan khong va co bing nita tdi gin kho, rdi hoa
tan lai trong 1ml hdn hgp
DCM/hexan
(l:3,v/v). Diing pipet Paster dua qua cot sic ky
dugc nhdi 5g cha't ha'p phu florisil (da hoat hoa 12 gid tai
130°C)
de tie'n hanh budc lam
sach. Thuc hien cac phan doan rira giai vdi lan lugt cac hon hgp dung mdi sau: 20ml
hexan/DCM
(l:3,v/v), 20ml hexan/DCM (2:3.v/v), 100ml 5% MeOH/ DCM. Phan
doan 3 chiia cac hgp chat ankylphenol va bisphenol A quan tam. Co cat quay chan
khong dich rira giai phan doan thu thap vl 1ml. Chuyin vao

<lml.
Them
10|il
chat npi
chuan naphtalen-d8
lOppm.
Dinh
miic
vl 1ml bing hexan. Chuyin sang
Ip
sic ky
1,5ml va tien hanh xac dinh tren GC/MS theo chuang trinh da dinh.
IV: KET QUA VA THAO LUAN
4.1.
Ket qua qua trinh din xuat hoa
Ky thuat dan xuat cd nhilu uu
diim
cho viec phat hien ddng thdi cac hgp chat
phenol vdi dp nhay va dp chpn Ipc cao. Trong dd cac ky thuat silyl hda dugc
iing
dung
rpng rai do cd kha nang cai thien dp chfnh xac, dp nhay, dp lap lai va kha nang phan
giai vi nd lam triet tieu duoi pic, tang tfnh
bin
nhiet
ciia
cac phenol. Tuy nhien gia
thanh cua chiing lai rat dit, khdng phu hgp vdi dilu kien nghien
ciiu
tai Viet Nam.

(san pham
ciia
phan
iing)
va anhidrite axetic du cd kha nang an mdn cac thiet bi kim
loai cua he thdng sic ky nen cin tien hanh loai bd chiing trudc khi bam len may.
H,C
C=0
o
CH3C00 +
H3C
H3C
o
R
C
I
o
c—o
0—(x
R
Hinh
6: Ca che phdn
I'ing
ddn
xudt axetyl hoa cacphenol.
4.2.
Xac dinh phan manh dac trung cua cau tu can phan
tich
Tien hanh bam
l|al

Dp phan
cue
cua dung moi rira giai cd
thi
anh hudng tdi hieu suat thu hdi
ciia
chat phan tfch trong miu moi trudng. Vdi cac mau
nude,
diclometan dugc chpn la dung
mdi chiet
bdd
chiing cd kha nang tuang tac manh vdi dang phenoxi tuang ddi phan
cue
trong moi trudng
pH=
2. Tuy nhien,
nude
rac la moi trudng rat phuc tap, chiia nhieu
cha't anh hudng nhu cha't mau, rugu, amin, axit hiiu ca. Bdi vay chiing toi da tien hanh
rira giai 3 phan doan nham muc dfch loai bd tdi da cac chat ban.
Ndng dp cac phenol dugc tfnh theo cong thiic:
C = Cspike - Cblank
Trong dd: Cspike : ndng dp cac phenol trong miu them chuin
Cblank: ndng dp cac phenol trong miu tring
Ket qua khao sat hieu suit thu hdi trung binh qua cot florisil tai ndng dp cac
phenol la 200ng/L sau 5 lin lap lai dugc trinh bay trong bang 5
Bdng 5: Ket qud phdn tich cdc phdn dogn rua gidi
Phan doan
FI
F2

-
-
193,6
2,2
-
BPA-
dl4
-
-
195,0
-
-
FI
n-hexane: DCM (1:3)
F2 n-hexane: DCM (2:3)
F3
DCM:
MeOH (95:5)
Qua khao sat nhan thay, vdi
thi
tfch cua 2 phan doan
FI,
F2 sir dung cac hdn
hgp dung moi n-hexane: DCM (1:3) va n-hexane: DCM (2:3) dl loai bd cae hgp chat
gay anh hudng ft phan cue han so vdi cac phenol ta thay cac hgp chat can phan tfch
chua bi rira giai ra. Va vdi
thi
tfch 100ml hdn hgp DCM: MeOH (95:5), cac phenol
dugc rira giai het. Vi vay, chiing toi chpn:
4-