Nghin cu phng php xc nh cc axit

bo trong mt s loi du m ng, thc vt

Vit Nam bng k thut sc k


V Th Vit Dung


Trng i hc Khoa hc T nhin
Lun n TS. ngnh: Ha phn tch; M s: 62 44 29 01
Ngi hng dn: PGS.TS. Nguyn Xun Trung, PGS. TS. Lu Vn Bi
Nm bo v: 2012


Abstract. S dng phng php quy hoch ha thc nghim - xy dng m hnh
hi quy bc hai tm trc giao tm iu kin ti u cho qu trnh xc nh cc axit
bo trong du m ng thc vt. Kt qu nghin cu thu c ti u hn nhiu
so vi cc nghin cu phn tch axit bo trc y. s dng cc k thut sc k
hin i: sc k kh ion ha ngn la (GC/FID) v sc k lng siu nhanh (UFLC)
phn tch ng thi 37 metyl este axit bo trong hn hp. Cc nghin cu c
tin hnh mt cch c h thng t kho st n l n m hnh ha cc yu t c nh
hng tng h. Qu trnh x l thng k v xc nhn gi tr s dng ca phng
php nghin cu c tin hnh y , p ng yu cu khi xy dng phng php
phn tch. ng dng phng php nghin cu xc nh cc axit bo trong 8 mu du
m ng thc vt thng dng ca Vit Nam gm: m c basa, m ln, du m, du
u nnh, du lc, du da, du ht cao su v du ht jatropha. Phn tch xut c
kh nng xy dng thnh phng php tiu chun xc nh thnh phn cc axit
bo trong du m ng thc vt, phc v nghin cu v dinh dng, kim nghim
thc phm, ch to nhin liu sinh hc v cc nghin cu khc.

Keywords. Ha phn tch; Axit bo; K thut sc k; Du ng vt; Du thc vt


Content
M U
1. Tnh cp thit ca lun n
Du m ng, thc vt (DMTV) ng vai tr to ln trong vic cung cp dinh dng
thit yu cho c th sng di dng thc n, thc phm chc nng, lm nguyn liu ch bin
thc n gia sc, nguyn liu sn xut nhin liu sinh hc (biodiesel),
Di dng thc phm thit yu, nu s dng v tiu th DMTV ng cch, ng hm
lng cht bo s cn bng c dinh dng v kim sot bnh tt. Vi cc loi DMTV c
hm lng dinh dng thp, du m thi hoc qua s dng, DMTV khng n c nh
du ht jatropha, ht cao su, thu du, to, c th s dng lm nguyn liu sn xut
biodiesel. y c xem l ngun nng lng thay th y tim nng.
Trn c hai phng din l thc phm dinh dng v nhin liu sinh hc th ti Vit
Nam hin cha c c s d liu y v hm lng cc axit bo trong du m ng, thc
vt. Cc quy trnh phn tch cng b v p dng ch yu t ti liu tham kho ca nc
ngoi. Cc s liu phn tch hm lng axit bo khng y , nn kh so snh nh gi ton
din ngun cung cp axit bo cho nhu cu lm thc phm hoc cho nguyn liu sn xut
nhin liu sinh hc.
V vy ti: Nghin cu phng php xc nh cc axit bo trong mt s loi du m
ng, thc vt Vit Nam bng k thut sc k s gip cho vic hon thin quy trnh phn
tch axit bo, p ng c yu cu phn tch cho cc phng th nghim u ngnh ti Vit
Nam.
2. Mc tiu v ni dung nghin cu
Mc tiu ca ti l nghin cu tng i ton din cc vn lin quan n qu trnh
tch v xc nh ng thi cc axit bo trong hn hp, qu trnh chuyn i DMTV thnh
metyl este axit bo (FAME) lm c s khoa hc tch v xc nh cc axit bo trong 8 mu
DMTV Vit Nam. T xy dng phng php tiu chun xc nh hm lng cc axit
bo trong DMTV nc ta.
Do ni dung ca lun n gm:
- Xy dng m hnh th nghim bc hai tm trc giao xt nh hng ng thi cc yu t
n kh nng tch v xc nh cc FAME bng phng php sc k kh.
- Da trn m hnh th nghim trn ti u ha v nh gi nh hng cc nhn t kho
st n vic tch v xc nh cc FAME bng phng php sc k kh detector ion ha ngn
la (GC/FID)
- S dng h thng sc k lng siu nhanh (UFLC) nghin cu tm iu kin ti u v
nh gi nh hng ng thi cc nhn t kho st n hiu sut qu trnh chuyn i este
du m.
- Xc nhn gi tr s dng ca phng php nghin cu.
- ng dng phng php nghin cu xc nh cc axit bo trong 8 mu DMTV Vit
Nam.
3. Nhng im mi v khoa hc ca lun n
3.1. Ln u tin Vit Nam s dng phng php quy hoch ha thc nghim theo m
hnh th nghim bc hai tm trc giao nghin cu nh hng ng thi cc yu t nh tc
pha ng, nhit ban u ca ct tch, tc tng nhit, t l bm chia dng n kh nng
tch v xc nh cc FAME bng phng php sc k kh vi detector ion ha ngn la.
- Ln u tin xy dng m hnh th nghim bc hai tm trc giao xt nh hng ng
thi cc yu t n hiu sut qu trnh chuyn i este DMTV nh t l mol metanol/du
m, hm lng cht xc tc (axit hoc kim), nhit , thi gian v mi trng phn ng
nhm t hiu sut chuyn i ti u (~ 100%).
3.2. Da trn cc iu kin ti u ha trn ln u tin tch v xc nh ng thi
37 FAME trong hn hp vi lp li tt, lm c s tin hnh xc nh cc axit bo trong
DMTV.
3.3. tin hnh nghin cu mt cch c h thng cc yu t nh hng n vic tch,
xc nh cc axit bo trong DMTV bng phng php sc k kh. Kt qu phn tch cc
axit bo x l thng k, xc nhn gi tr s dng ca phng php, p ng yu cu khi
xy dng phng php phn tch.
3.4. Ln u tin tin hnh phn tch ng thi cc axit bo trong 8 mu DMTV
Vit Nam: m c basa, m ln, du m, du u nnh, du lc, du da, du ht cao su v
du ht jatropha.
3.5. Phng php phn tch xut c kh nng xy dng thnh phng php tiu chun
xc nh thnh phn axit bo trong DMTV Vit Nam.
4. B cc ca lun n
Lun n gm 151 trang vi 42 bng s liu, 37 hnh v, 178 ti liu tham kho v 11
phn ph lc c chia thnh cc phn nh sau: m u: 2 trang, chng 1. tng quan ti
liu: 31 trang, chng 2. thc nghim v phng php nghin cu: 23 trang, chng 3. kt
qu v tho lun: 74 trang, kt lun v kin ngh: 2 trang, ti liu tham kho: 18 trang.


Chng 1. TNG QUAN

Chng ny tng hp l thuyt v cht bo v axit bo, cc cng trnh nghin cu Vit
Nam v nc ngoi v cc phng php nh lng cht bo v axit bo, cc phng php
iu ch v cc yu t nh hng n qu trnh iu ch FAME, phng php quy hoch ha
thc nghim tm iu kin ti u tch v xc nh cc axit bo.


Chng 2. THC NGHIM V PHNG PHP NGHIN CU

2.1. Nguyn liu, ha cht v thit b th nghim
Nguyn liu DMTV c la chn nghin cu gm: M c basa An Giang do Cng
ty c phn xut nhp khu thy sn An Giang (Agifish) cung cp, m ln t cc ch H Ni,
c nu chy thnh dng du, du u nnh, du m, du lc, du da t Hp tc x Nng
nghip Qung Ngi, du c p t ht u nnh, ht m, ht lc v cm da Qung Ngi,
du ht cao su v du ht jatropha t cng ty Sn xut Xut nhp khu Bnh Dng, du
c p t ht cao su v ht jatropha k Nng.
Cht chun v ni chun ca Sigma (M), dung mi loi phn tch ca Merck (c), cc
ha cht khc: CH
3
OH cng nghip 90% (Malaysia), KOH 82%, NaOH 96%, H
2
SO
4

96% (Trung Quc),
Thit b s c ky

lng siu nhanh UFLC ca Shimadzu (Nht) vi detector ch s khc x

RID10A, my sc k lng: LC20AD, degasser: DGU20A
3
, l ct: CTO20A, ct sc k:
Cadenzal CDC18 (250 mm 4,6 mm ID 3 m) ca Imtakt (M); thit b sc k kh
Shimadzu GC2010 (Kyoto, Nht) vi detector FID, ct mao qun phn cc mnh SP
TM
-
2560 (100 m 0,25 mm 0,2 m) v ct mao qun t phn cc Equity-5 (30 m 0,25 mm
0,25 m) ca Supelco (M), my khuy t gia nhit Velp 1200 rmp (Italia), l vi sng Sanyo
1200W (Nht), bm chn khng IKA (c), my rung siu m Telsonic 750W (Thy S),...
2.2. Phng php nghin cu
2.2.1. Tch v xc nh cc FAME
S dng sc k kh vi detector FID, ct mao qun phn cc mnh SP
TM
-2560 (100 m
0,25 mm 0,25 m) c thnh phn 100% poly(xyanoisopropyl siloxan), kh mang Heli, dung
mi diclometan, ni chun n-hexadecan.
2.2.2. Xc nh hm lng axit bo t do trong du m
S dng phng php chun vi dung dch NaOH 0,01M, ch th phenolphatalein.
2.2.3. Chuyn i este du m ng thc vt
S dng phn ng transeste ha DMTV vi metanol xc tc kim v phn ng este
ha DMTV vi metanol xc tc axit.
2.2.4. Xc nh mc chuyn i este
S dng sc k lng siu nhanh vi ct sc k Cadenzal CDC18 (250 mm 4,6 mm
3 m), detector: RID10A, nhit l ct: 35
0
C, pha ng: Ace/ACN (7/3; v/v), tc : 0,5
ml/pht, th tch tim mu: 25l.
2.2.5. Thu thp mu phn tch
S dng phng php ly mu DMTV theo TCVN 2625:2005 (hay ISO 05555:2001).
2.2.6. Nghin cu tm iu kin ti u cho qu trnh tch v xc nh cc axit bo
S dng phng php mt mc tiu theo m hnh hi quy bc hai tm trc giao vi s
h tr ca phn mm Modde 5.0.
2.2.7. nh gi thng k phng php phn tch
Thng qua vic xy dng ng chun, tnh sai s, nhy, lp li, ng, hiu
sut thu hi v so snh kt qu phn tch vi kt qu kim nghim Vilas (ISO 17025:2005).


Chng 3. KT QU V THO LUN

3.1. Nghin cu ti u ha iu kin GC/FID xc nh cc FAME
3.1.1. Ti u ha iu kin GC/FID theo phng php n bin
Trc ht chng ti kho st, so snh kh nng tch cc FAME ( phn gii R) v
lp li ( lch chun tng i RSD%) v t l din tch pic cc FAME/IS la chn loi
ct tch (ct mao qun phn cc mnh SP
TM
-2560) v loi kh mang (kh He) c nh dng
cho GC/FID do trong qu trnh phn tch vic thay i hai nhn t ny gp nhiu kh khn.
nhy, n nh ( lp li) ca h thng phn tch thay i ng k khi thay i hai yu
t ny. Sau chng ti tip tc kho st xc nh khong bin thin cc iu kin phn tch
ca GC/FID ti u ha cc iu kin ny nhm tch tt cc FAME. Kt qu kho st n
bin tm khong bin thin cc iu kin phn tch GC/FID thu c nh sau:
- Tc pha ng (tc kh mang) He: 18 25 cm/s
- Tc tng nhit ca ct tch: 2 4
0
C/pht
- Nhit ban u ca ct tch: 60 140
0
C
- T l bm chia dng: 10:1 200:1
3.1.2. Ti u ha iu kin GC/FID theo phng php a bin
3.1.2.1. Xy dng m hnh hi quy bc hai tm trc giao
S dng m hnh hi quy bc hai tm trc giao xy dng phng trnh hi quy
(PTHQ) v nh gi nh hng ng thi ca 4 nhn t kho st: tc pha ng, X
1
; nhit
ban u ca ct tch, X
2
; tc tng nhit ca ct tch, X
3
; t l bm chia dng, X
4
n
kh nng tch ( phn gii R) cc FAME, y
1
v lch chun tng i (RSD%) ca t l
din tch pic FAME/IS, y
2
. Kt qu thc nghim c trnh by trn bng 3.2.
Quan h gia hm mc tiu v cc nhn t kho st c m t theo phng trnh bc
hai: y = b
0
x
0
+ b
1
x
1
+ ...

+ b
12
x
1
x
2
+ b
13
x
1
x
3
+ ...+ b
11
(x
1
2
) + b
22
(x
2
2
) + Vi tham s
hi quy v cnh tay n sao d c tnh sn cho m hnh hi quy bc hai tm trc giao khi
n = 4 l: = 0,8000, d = 1,4142.
Bng 3.2. Kt qu thc nghim tm iu kin GC/FID tch v xc nh cc FAME theo m
hnh hi quy bc hai tm trc giao
TT
Bin m ha Bin s thc Kt qu
x
1
x
2
x
3
x
4
X
1
X
2
X
3
X
4
y
1
y
2
1 -1 -1 -1 -1 18 60 2 10
0,5
9
1,76
2 1 -1 -1 -1 25 60 2 10 0,6 1,88
3 -1 1 -1 -1 18 140 2 10
1,0
2
1,75
4 1 1 -1 -1 25 140 2 10
0,2
1
1,79
5 -1 -1 1 -1 18 60 4 10 0 1,92
6 1 -1 1 -1 25 60 4 10 0 1,79
7 -1 1 1 -1 18 140 4 10
0,4
3
1,69
8 1 1 1 -1 25 140 4 10 0 1,75
9 -1 -1 -1 1 18 60 2 200 0,6 3,85
2
10 1 -1 -1 1 25 60 2 200
0,1
7
3,92
11 -1 1 -1 1 18 140 2 200
1,0
9
3,82
12 1 1 -1 1 25 140 2 200
0,2
4
3,88
13 -1 -1 1 1 18 60 4 200 0 3,84
14 1 -1 1 1 25 60 4 200 0 3,87
15 -1 1 1 1 18 140 4 200
0,4
7
3,84
16 1 1 1 1 25 140 4 200 0 3,92
17
-
1,4142
0 0 0 16,6 100 3 105
0,7
8
3,23
18 1,4142 0 0 0 26,4 100 3 105
0,1
5
3,18
19 0
-
1,4142
0 0 21,5 43,4 3 105
0,6
8
3,2
20 0 1,4142 0 0 21,5 156,6 3 105
0,9
9
3,23
21 0 0
-
1,4142
0 21,5 100 1,6 105
0,6
6
3,16
22 0 0 1,4142 0 21,5 100 4,4 105 0 3,19
23 0 0 0
-
1,4142
21,5 100 3 -29,3
- -
24 0 0 0 1,4142 21,5 100 3
239,
3
0,8
6
4,07
25
1
0 0 0 0 21,5 100 3 105
0,9
6
3,24
25
2
0 0 0 0 21,5 100 3 105
0,9
6
3,19
25
3
0 0 0 0 21,5 100 3 105
0,9
7
3,23

y, cn tin hnh N = 27 th nghim xc nh cc h s trong PTHQ. Th nghim
th 25 l th nghim tm c tin hnh 3 ln. Phng sai ca cc th nghim c xc
nh theo th nghim b sung tm l
2
0(R)
S = 7,43.10
-5
,
2
0(RSD)
S = 7.10
-4
. T kt qu th nghim,
s dng phn mm Modde 5.0 loi b cc h s hi quy khng ph hp, tc l cc h s c
TN
i
t =
i
i b
b / S < t
p
(f) hay
TN
i
t < t
(0,05)
(2) = 4,3. Kt qu c ch ra trn bng 3.3.
Bng 3.3. Kt qu phn tch nh hng ca cc nhn t kho st n kh nng tch cc
FAME (I) v lch chun tng i ca t l din tich pic FAME/IS (II) ca GC/FID theo
m hnh hi quy bc hai tm trc giao
y
H s hi quy Phng sai mu Chun t
tin cy
()
I II I II I II I II
b
0
0,95 3,24 1,42.10
-16

8,01.10
-
19
8,0.10
7
3,6.10
9

0,03 0,06
x
1
-0,22 0,01 3,89.10
-13
0,30 3,7.10
5
0,018 0,01 0,03
x
2
0,12 -0,02 2,84.10
-10
0,17 7,0.10
3
0,049 0,01 0,03
x
3
-0,21 6,00.10
-4
6,10.10
-13
0,96 2,7.10
5
6,1.10
-4
0,01 0,03
x
4
0,01 1,04 0,12
1,45.10
-
16
0,024 8,6.10
7

0,01 0,03
x
1
.x
1
-0,24 -0,02 2,36.10
-11
0,29 4,9.10
4
0,037 0,02 0,04
x
2
.x
2
-0,05 -0,02 8,71.10
-5
0,41 5,7 0,031 0,02 0,04
x
3
.x
3
-0,31 -0,04 1,50.10
-12
0,08 2,5.10
5
0,14 0,02 0,04
x
4
.x
4
-0,05 -0,33 1,19.10
-5
1,15.10
-8
13 3,1.10
-3
0,02 0,05
x
1
.x
2
-0,11 0,01 3,17.10
-9
0,49 1,9.10
3
0,014 0,01 0,03
x
1
.x
3
0,10 -0,02 3,99.10
-9
0,26 1,6.10
3
0,039 0,01 0,03
x
1
.x
4
-0,01 0,01 0,30 0,49 0,013 0,014 0,01 0,03
x
2
.x
3
-0,01 3,10.10
-3
0,20 0,82 0,02 3,4.10
-3
0,01 0,03
x
2
.x
4
0,01 0,02 0,38 0,13 9,7.10
-3
0,056 0,01 0,03
x
3
.x
4
-0,01 1,90.10
-3
0,31 0,89 0,013 2,0.10
-3
0,01 0,03
N = 26
2
I
R = 0,9983 RSD
I
=0,025
P =0,95
2
II
R = 0,9984 RSD
II
=0,053
*Ghi ch: Nhng h s in nghing, m l h s khng c ngha trong PTHQ.

Nhng kt qu thu c bng 3.3 cho thy c nh hng bc nht ti kh nng tch
cc FAME y
1
l tc pha ng x
1
(tiu cc), nhit ban u x
2
(tch cc) v tc tng
nhit ca ct tch x
3
(tiu cc), cn t l bm chia dng x
4
th nh hng khng ng k.
Ngc li t l bm chia dng li l nhn t bc nht nh hng ch yu (tch cc) n
lch chun tng i ca t l din tch pic FAME/IS y
2
, ba nhn t cn li th t nh hng.
Kh nng tch cc FAME chu nh hng tiu cc bc hai ca c bn nhn t kho st v
nh hng ng thi ca tc pha ng v nhit ban u ca ct tch, x
1
x
2
(tiu cc),
tc pha ng v tc tng nhit ca ct tch, x
1
x
3
(tch cc). Trong khi lch chun
tng i ca t l din tch pic FAME/IS ch chu nh hng bc hai ca t l bm chia
dng, x
4
2
(tiu cc), nh hng bc hai v nh hng ng thi ca cc nhn t khc l
khng ng k.
T kt qu thu c trn bng 3.3, sau khi loi nhng nhn t khng ph hp, c th vit
c PTHQ dng m ha m t s ph thuc ca y
1
, y
2
vo cc nhn t x
i
nh sau:
y
1
= 0,95 0,22x
1
+ 0,12x
2
0,21x
3
0,11x
1
x
2
+ 0,10x
1
x
3
0,24(x
1
2
0,800) 0,05(x
2
2

0,800) 0,31(x
3
2
0,800) 0,05(x
4
2
0,800) (3.1)
y
2
= 3,24 + 1,04x
4
0,33(x
4
2
0,800) (3.2)
S dng chun Fisher kim tra s ph hp ca m hnh:
F
m hnh I
=
I
2
ph hp I
2
0
S
S
=
4
5
4, 53.10
6, 09
7, 43.10

= < F
bng
= F
0,95
(15, 2) = 19,43.
F
m hnh II
=
II
2
ph hp II
2
0
S
S
=
3
4
1, 33.10
1, 91
7.10

= < F
bng
= F
0,95
(23, 2) = 19,45.
F
m hnh
< F
bng
: m hnh thng k m t ng thc nghim.
Do m hnh ton hc m t quan h gia kh nng tch cc FAME v lch chun
tng i ca t l din tch pic FAME/IS vo cc bin thc nh sau:
Y
1
= -8,67 + 0,76X
1
+ 0,03X
2
+ 0,99X
3
+ 0,01.10
-1
X
4
0,75.10
-3
X
1
X
2
+ 0,03X
1
X
3

0,02X
1
2
0,33.10
-4
X
2
2
0,31X
3
2
0,05.10
-4
X
4
2
(3.3)
Y
2
= 1,95 + 0,02X
4
3,65.10
-5
X
4
2
(3.4)
Vi
o
i i
i
i
X X
x

=

. Trong : X
i
: cc gi tr dng thc ca nhn t kho st,
o
i
X : mc gc
(0) ca X
i
, x
i
: cc gi tr m ha ca X
i
,
i
: khong bin thin X
i
.
Hai PTHQ trn phn nh kh chnh xc m hnh thc nghim, iu ny c khng
nh qua cc gi tr lch chun R
2
ca m hnh (bng 3.3). M hnh c th d on kh
nng tch cc FAME v lch chun tng i ca t l din tch pic FAME/IS vi
chnh xc cao, tng ng l 99,83% v 99,84%, gia gi tr thu c t m hnh d on v
gi tr thc nghim ch c mt s sai khc nh.
3.1.2.2. Xc nh iu kin ti u ca GC/FID
Da trn m hnh hi quy bc hai tm trc giao xy dng c khi thc nghim kho st
nh hng ng thi ca cc nhn t ca GC/FID n kh nng tch cc FAME v lch
chun tng i ca t l din tch pic FAME/IS xc nh iu kin ti u. Bng cch ly
o hm ca hm hi quy theo tng bin v cho bng 0 tm ra cc tr ca hm (thng qua
phn mm Modde 5.0) tm c iu kin ti u tch v xc nh cc FAME nh sau: tc
kh mang He: 20,5 cm/s; tc tng nhit ca ct tch: 2,4
0
C/pht; nhit ban u ca
ct tch: 140
0
C; t l bm chia dng: 30:1. iu kin ti u trn, kh nng tch cc FAME
v lch chun tng i ca t l din tch pic FAME/IS c gi tr d on theo m hnh
ti u ha ln lt l 1,08 v 2,11%. Cc gi tr trung bnh tng ng thu c khi tin hnh
thc nghim 3 ln vi cht chun FAME 204060 ppm l 1,08 v 2,12%.
Gi tr cc phng sai thc nghim theo iu kin ti u thu c:
I
2
tu
S = 6,43.10
-5
,
II
2
tu
S =
5,33.10
-4
v ca m hnh tng ng l:
I
2
0
S = 7,43.10
-5
,
II
2
0
S = 7,00.10
-4
. C F
tnh I
= 7,43.10
-
5
/6,43.10
-5
= 1,16; F
tnh II
= 7,00.10
-4
/5,33.10
-4
= 1,31 < F
bng
(0,95; 2; 2) = 19. Nh vy
chnh xc ca cc s liu theo m hnh v theo thc nghim iu kin ti u l ging nhau.
Kt qu ny cho thy m hnh d on c chnh xc cao, m bo tin cy. y l mt
cng c hu ch trong vic tin on kt qu cng nh ti u ha cc iu kin thc nghim.
3.2. Nghin cu chuyn i DMTV thnh FAME
3.2.1. Kim tra hm lng axit bo t do, la chn quy trnh chuyn i
Hm lng axit bo t do (%FFA) c nh hng n quy trnh chuyn i DMTV
thnh FAME. Cc phn ng chuyn i este dng xc tc kim cn c nguyn liu u vi
hm lng FFA < 2,5%. Nu hm lng FFA > 2,5% th cn s dng nhiu kim hn
trung ha FFA, ng thi sn phm to ra x phng v nc nhiu hn. X phng sinh ra lm
tng nht ca hn hp, to thnh nh v lm cho vic tch glyxerin tr nn kh khn.
Phn ng sinh ra nhiu nc c th lm cho metyl este b thy phn to ra axit bo v
metanol, do vy tiu tn nhiu xc tc hn v hiu sut phn ng b gim i ng k. Do
vi du m c hm lng FFA > 2,5% cn chuyn i qua hai giai on, giai on u thc
hin phn ng este ha xc tc axit chuyn axit bo t do thnh FAME sau tip tc giai
on hai vi phn ng transeste ha du m s dng xc tc kim. V vy trc ht chng ti
chun kim tra hm lng axit bo t do ca nguyn liu DMTV la chn quy trnh
chuyn i DMTV thnh FAME thch hp.
Kt qu phn tch cho thy hm lng FFA trong m c basa: 1,26%; m ln: 0,45%;
du u nnh: 0,21%; du m: 1,68%; du lc: 0,33% v du da: 0,21%. Cc mu du m
ny u c hm lng FFA < 2,5%, hon ton thch hp tin hnh chuyn i thnh FAME
bng phng php metyl este ha xc tc kim mt giai on. Ring du ht cao su v du
ht jatropha c hm lng FFA rt ln, tng ng 46,19% v 21,01%, phi tin hnh chuyn
i qua hai giai on, giai on u este ha vi xc tc axit, giai on hai chuyn v este vi
xc tc kim.
3.2.2. iu kin chuyn i este theo phng php n bin
Qua kho st n bin cc nhn t nh hng n hiu sut phn ng chuyn i este
gia m c basa v metanol s dng xc tc kim v c mt ca dung mi chng ti thu c
khong bin thin cc iu kin phn ng nh sau:
+ T l mol metanol/m c (X
1
, mol/mol)): 4/1 7/1;
+ Nng xc tc KOH (X
2
, % m/m): 0,75 1,25%;
+ Nhit phn ng (X
3
,
0
C): 30 60
0
C;
+ Thi gian phn ng (X
4,
pht): 10 40 pht.;
+ Hm lng dung mi axeton (X
5
, % m/m): 10 30%.
Kt qu kho st n bin cc nhn t nh hng n hiu sut phn ng este ha xc
tc axit (giai on 1) ca qu trnh chuyn i 2 giai on iu ch FAME t du ht cao su
thu c khong bin thin cc nhn t nh sau (tt c cc phn ng u thc hin nhit
si ca hn hp, ~ 60
0
C):
+ T l mol metanol/du (X
1
, mol/mol): 3/1 9/1
+ Hm lng xc tc H
2
SO
4
(X
2
, % m/m): 0,5 2%
+ Thi gian phn ng (X
3,
gi): 1 6 gi
+ Hm lng dung mi axeton (X
4
, % m/m): 10 50%
3.2.3. iu kin chuyn i este theo phng php a bin
* Xy dng m hnh hi quy bc hai tm trc giao
Tng t nh qu trnh thc nghim ti u ha cc iu kin GC/FID tch v xc
nh cc FAME, vi qu trnh chuyn i DMTV, qua m hnh hi quy bc hai tm trc
giao, chng ti thu c cc PTHQ dng m ha sau khi loi b cc nhn t nh hng
khng ng k nh sau:
- Hiu sut phn ng este ha xc tc kim iu ch FAME t m c basa ( = 0,7698):
y
1
= 94,06 + 5,88x
1
+ 1,53x
2
+ 2,18x
3
+ 4,46x
4
+ 0,99x
5
0,80x
1
x
2
0,77x
1
x
3
0,71x
1
x
4

4,76x
4
2
+ 0,96x
5
2
(3.5)
- Hiu sut phn ng este ha xc tc axit (giai on 1) ca qu trnh chuyn i hai giai
on iu ch FAME t du ht cao su ( = 0,8000):
y
2
= 105,36 + 9,24x
1
+ 3,61x
2
+ 3x
3
+ 2,08x
4
1,18x
1
x
2
1,04x
1
x
4
1,47x
2
x
3
11,08x
1
2

3,2x
4
2
(3.6)
Bin i
o
i i
i
i
X X
x

=

a phng trnh (3.5) v (3.6) v dng thc tng ng l :

Y
1
= 38,41 + 7,18X
1
+ 7,88X
2
+ 0,30X
3
+ 1,60X
4
0,28X
5
1,07X
1
X
2
0,03X
1
X
3

0,04X
1
X
4
0,03X
4
2
+ 0,01X
5
2
(3.7)
Y
2
= 20,39 + 17,71X
1
+ 4,43X
2
+ 2,18X
3
+ 0,68X
4
0,52X
1
X
2
0,02X
1
X
4

0,78X
2
X
3
1,23X
1
2
0,01X
4
2
(3.8)
Kt qu phn tch cho thy c nh hng tch cc nht bc 1 n hiu sut phn ng
chuyn i m c basa thnh FAME l t l mol metanol/m c (x
1
), tip n l thi gian
phn ng (x
4
), nhit phn ng (x
3
), hm lng xc tc (x
2
) v hm lng dung mi (x
5
) t
nh hng nht. nh hng tiu cc nht bc hai n hiu sut phn ng l nhn t thi
gian (x
4
2
). nh hng bc hai ca t l mol metanol/m c (x
1
2
), hm lng xc tc (x
2
2
),
nhit phn ng (x
3
2
) v nh hng ng thi ca t l mol metanol/m c v hm lng
dung mi (x
1
x
5
), hm lng xc tc v nhit phn ng (x
2
x
3
), hm lng xc tc v thi
gian phn ng (x
2
x
4
), hm lng xc tc v hm lng dung mi (x
2
x
5
), nhit phn ng v
thi gian phn ng (x
3
x
4
), nhit phn ng v hm lng dung mi (x
3
x
5
), thi gian phn
ng v hm lng dung mi (x
4
x
5
) n hiu sut phn ng l khng ng k. S tng ng
thi ca t l mol metanol/m c vi hm lng xc tc (x
1
x
2
), vi nhit phn ng (x
1
x
3
)
v vi thi gian phn ng (x
1
x
4
) u lm gim hiu sut phn ng (nh hng tiu cc). Kt
qu ny c th hin trn hnh 3.14.

Hnh 3.14. nh hng ca cc nhn t kho st n hiu sut phn ng chuyn i este xc
tc kim m c basa
i vi qu trnh chuyn i hai giai on, kt qu phn tch cho thy c bn nhn t
kho st u nh hng tch cc bc 1 n hiu sut phn ng este ha xc tc axit du ht
cao su trong t l mol metanol/du (x
1
) c nh hng tch cc nhiu nht, tuy nhin s
tng ng thi t l metanol/du (x
1
x
1
) li lm gim nhiu nht hiu sut phn ng (nh
hng tiu cc). Cc nh hng bc hai v nh hng ng thi ca cc nhn t kho st
cng u l nh hng tiu cc. S thay i ng thi hm lng xc tc (x
2
x
2
), thi gian
phn ng (x
3
x
3
), t l mol metanol/du v thi gian phn ng (x
1
x
3
), xc tc v dung mi
(x
2
x
4
), thi gian phn ng v dung mi (x
3
x
4
) t nh hng n hiu sut phn ng. nh
hng ca cc nhn t kho st n hiu sut phn ng este ha du ht cao su c th hin
trn hnh 3.17.
Hnh 3.17. S bin thin ca hiu sut phn ng este ha xc tc axit du ht cao su theo t
l mol metanol/du (3/1 9/1) v hm lng dung mi (10 50%) khi c nh hm lng
xc tc (1,25%) v thi gian phn ng (3,5 gi).

Kt qu nghin cu cng cho thy tng quan gia hiu
sut phn ng chuyn i este m c basa thnh FAME thu c
t thc nghim v tnh ton t PTHQ l 99,7%, ca phn ng este
ha xc tc axit du ht cao su l 98,7%. Nh vy gia gi tr thu
c t m hnh d on v gi tr thc nghim ch c mt s sai
khc nh.
* Xc nh iu kin ti u
Da trn PTHQ xy dng c, vi s h tr ca phn mm Modde 5.0, bng phng
php o hm tm c iu kin ti u ca qu trnh chuyn i DMTV thnh FAME t
m c basa: t l mol metanol/m c: 6/1 (mol/mol); nng xc tc KOH: 0,98% (m/m);
nhit phn ng: 37,8
0
C; thi gian phn ng: 23,5 pht; hm lng dung mi axeton: 30%
(m/m). iu kin ti u ny, hiu sut chuyn i mt giai on cc FAME d on c gi
tr l 99,9%, gi tr tng ng thu c khi tin hnh thc nghim lp li ba ln vi mu m
c basa l 99,7%. Gi tr phng sai theo iu kin ti u thu c l S
tu
2
= 0,0233, theo m
hnh l S
0
2
= 0,0351, F
tn
= 0,0351/0,0233 = 1,51 < F
bng
(0,95, 2, 2) = 19, vy chnh xc
ca cc s liu theo m hnh v theo thc nghim iu kin ti u l ging nhau.
iu kin ti u ca phn ng este ha xc tc axit (giai on mt) ca qu trnh hai giai
on iu ch FAME t du ht cao su thu c nh sau: t l mol metanol/du: 7,5/1
(mol/mol); hm lng xc tc H
2
SO
4
: 1,65% (m/m); thi gian phn ng: 4 gi; hm lng
dung mi axeton: 35%; phn ng thc hin 60
o
C. iu kin ti u ny, hiu sut phn
ng este ha d on c gi tr l 97,9%. Kt qu thc nghim thu c gi tr trung bnh ca
3 ln th nghim iu kin ny l 98,3%. Gi tr phng sai theo iu kin ti u thu c
l S
tu
2
= 0,034, ca m hnh l S
0
2
= 0,350, F
tn
= 0,350/0,034 = 10,29 < F
bng
(0,95, 2, 2) = 19,
chnh xc ca cc s liu theo m hnh v theo thc nghim iu kin ti u l ging
nhau.
Qua so snh kt qu nghin cu vi cc kt qu chuyn i este DMTV theo hng
kho st n bin tng nhn t vi cc loi xc tc khc nhau cho thy phn ng chuyn i
theo hng ti u ha ng thi cc nhn t trong mi trng ng th t c hiu sut
cao hn vi lng metanol cn dng t hn, thi gian ngn v nhit thp hn nhiu.
chnh l u im ca phng php ti u ha chuyn i DMTV thnh FAME ny so vi
cc nghin cu chuyn i trc y.
3.3. Xc nhn gi tr s dng ca phng php phn tch
3.3.1. Xy dng ng chun, xc nh gii hn pht hin v gii hn nh lng
tin hnh xy dng ng chun dng cho vic phn tch cc FAME, mt dy chun
hn hp 37 FAME c nng t 246 ppm n 50100150 ppm c tim vo h
GC/FID. T cc kt qu phn tch, v th s ph thuc t l din tch pic FAME/IS vo
nng ca cc FAME thu c cc ng chun tng ng. Da trn phng trnh ng
chun: y = ax + b tnh LOD theo cng thc:
B
LOD 3.S / b = , trong S
B
: lch chun ca
mu trng, nu khng lm th nghim vi mu trng th S
B
= S
y
( lch chun ca phng
trnh hi quy). LOQ = 3,3LOD. Kt qu phn tch c ch ra trn bng 3.16. T kt qu
phn tch cho thy c s tng quan tuyn tnh cht ch ca t l din tch pic FAME/IS vo
nng cc FAME (R > 0,999) v h thng phn tch GC/FID c nhy cao, pht hin
c cc FAME n 0,2 ppm v nh lng c n 0,7 ppm.
Bng 3.16. Phng trnh hi quy, gii hn pht hin, gii hn
nh lng cc FAME ca phng php phn tch
TT FAME Phng trnh hi quy ( P =0,95) R

LO
D
(pp
m)
LO
Q
(pp
m)
1 C4:0
y = (0,2138 0,0334)x (0,7961
1,6451) 0,9964 0,8 2,6
2 C6:0
y = (0,1066 0,0191)x (0,3036
0,9336) 0,9953 1,6 5,2
3 C8:0
y = (0,2688 0,0347)x (0,7646
1,7056) 0,9976 0,3 1,1
4 C10:0
y = (0,2776 0,0286)x (0,5932
1,4071) 0,9984 0,7 2,5
5 C11:0
y = (0,2595 0,0220)x (0,2424
0,5387) 0,9990 0,9 3,1
6 C12:0
y = (0,2646 0,0220)x (0,4430
1,0873) 0,9990 1,0 3,3
7 C13:0
y = (0,2505 0,0216)x (0,2174
0,5343) 0,9989 1,5 4,9
8 C14:0
y = (0,2599 0,0216)x (0,4558
1,0707) 0,9990 1,1 3,5
9 C14:1
y = (0,2466 0,0159)x (0,1023
0,3895) 0,9994 0,5 1,7
10 C15:0
y = (0,2512 0,0197)x (0,1922
0,4856) 0,9991 0,9 3,1
11 C15:1
y = (0,2322 0,0146)x (0,0498
0,3618) 0,9994 0,8 2,6
12 C16:0
y = (0,2581 0,0226)x (0,5489
1,6721) 0,9989 2,0 6,5
Bng 3.16. Phng trnh hi quy, gii hn pht hin, gii hn
nh lng cc FAME ca phng php phn tch
TT FAME Phng trnh hi quy ( P =0,95) R

LO
D
(pp
m)
LO
Q
(pp
m)
13 C16:1
y = (0,2546 0,0229)x (0,1097
0,5667) 0,9988 0,8 2,7
14 C17:0
y = (0,2229 0,0210)x (0,1632
0,5174) 0,9987 0,2 0,7
15 C17:1
y = (0,2373 0,0210)x (0,1194
0,5180) 0,9988 0,2 0,7
16 C18:0
y = (0,2436 0,0353)x (0,4954
1,7351) 0,9969 1,4 4,6
17
C18:1n-
9t
y = (0,2683 0,0382)x (0,3669
0,9365) 0,9970 0,8 2,7
18
C18:1n-
9c
y = (0,2485 0,0073)x (0,2644
1,1500) 0,9987 0,5 1,7
19
C18:2n-
6t
y = (0,2220 0,0185)x (0,1188
0,4499) 0,9990 0,5 1,8
20
C18:2n-
6c
y = (0,2246 0,0248)x (0,0773
0,6119) 0,9982 1,0 3,4
21 C20:0
y = (0,2428 0,0280)x (0,4469
1,3800) 0,9980 1,9 6,1
22 C18:3n-6
y = (0,2010 0,0150)x (0,0759
0,3701) 0,9992 0,8 2,6
23 C20:1
y = (0,2322 0,0239)x (0,1528
0,5855) 0,9985 0,9 2,9
24 C18:3n-3
y = (0,2017 0,0185)x (0,0941
0,4550) 0,9988 0,8 2,5
25 C21:0
y = (0,2784 0,0566)x (0,5429
1,3969) 0,9939 0,7 2,4
26 C20:2
y = (0,1954 0,0264)x (0,1625
0,6517) 0,9973 1,2 4,1
27 C22:0
y = (0,2326 0,0283)x (0,4390
1,3988) 0,9978 1,4 4,5
28 C20:3n-6
y = (0,2256 0,0296)x (0,2176
0,7242) 0,9975 0,4 1,4
29 C22:1n-9
y = (0,1910 0,0130)x (0,0107
0,3246) 0,9993 1,5 5,0
30 C20:3n-3
y = (0,2265 0,0267)x (0,1597
0,6545) 0,9980 1,0 3,2
31 C22:4n-6
y = (0,1847 0,0207)x (0,1544
0,5107) 0,9981 0,9 2,8
32 C23:0
y = (0,2001 0,0245)x (0,1093
0,6039) 0,9978 0,4 1,3
33 C22:2 y = (0,1528 0,0162)x (0,0829 0,9984 1,8 5,8
Bng 3.16. Phng trnh hi quy, gii hn pht hin, gii hn
nh lng cc FAME ca phng php phn tch
TT FAME Phng trnh hi quy ( P =0,95) R

LO
D
(pp
m)
LO
Q
(pp
m)
0,3962)
34 C24:0
y = (0,2274 0,0315)x (0,5378
1,5522) 0,9972 2,2 7,3
35 C20:5n-3
y = (0,2198 0,0178)x (0,1239
0,4398) 0,9990 1,9 6,3
36 C24:1
y = (0,1216 0,0140)x (0,0766
0,3449) 0,9980 0,8 2,5
37 C22:6n-3
y = (0,1994 0,0111)x (0,0331
0,2762) 0,9995 0,4 1,3
MIN 0,2
0,
7
MAX 2,2
7,
3

3.3.2. Kho st lp li
lp li ca h thng sc k kh (thi gian lu, t l din tch pic FAME/IS) c kho
st bng cch bm 7 ln song song mu chun hn hp 37 FAME 20-40-60 ppm trong cng
iu kin ti u ca GC/FID. Kt qu thu c cho thy lp li ca h thng sc k kh rt
tt, gi tr lch chun tng i v thi gian lu ca mu chun hn hp 37 FAME 20-40-
60 ppm dao ng trong khong t 0,03 n 0,08%, lch chun tng i v t l din tch
pic FAME/IS dao ng trong khong t 1,28 n 4,98%. Khi hm lng cht phn tch 10
ppm th RSD (%) cho php l 7,3%, hm lng cht phn tch 100 ppm th RSD (%) cho
php l 5,3% [117]. Nh vy vi mu chun FAME 20-40-60 ppm, lch chun tng i
ca h thng GC u di 5%, p ng c yu cu phn tch nh lng.
Kt qu kho st lp li 6 ln ca phng php phn tch khi tin hnh thc nghim
trn 8 mu DMTV Vit Nam cc iu kin ti u ca qu trnh chuyn i este v ca
GC/FID cho thy lch chun tng i v hm lng FAME iu ch t m c basa dao
ng t 1,02 n 4,65%, m ln: t 1,25 n 5,13%, du u nnh: t 0,87 n 5,18%, du
m t 1,18 n 4,72%, du lc: t 1,28 n 4,96%, du da: t 0,95 n 4,89%, du ht cao
su: t 0,95 n 4,96% v du ht jatropha: t 0,92 n 4,98%. Vi hm lng FAME o
c trong 8 mu DMTV dao ng t 0,178 n 433,471 mg/g th RSD (%) cho php ti
a l 5,3% [117]. Gi tr lch chun tng i cao nht thu c khi phn tch FAME l
5,18% trn mu du u nnh. Vy RSD% thu c khi phn tch cc FAME u < 5,3%, do
lp li ca phng php phn tch p ng c yu cu nh lng trong ha hc.
3.3.3. Xc nh ng v hiu sut thu hi
ng ca phng php phn tch c xc nh bng cch thm chun trn nn mu
trng. Hiu sut thu hi c xc nh bng cch thm chun trn nn mu thc. Cc mu
thc sau khi tin hnh nh lng FAME v bit c hm lng ca chng trong mu, thm
chnh xc mt lng chun FAME sao cho tng hm lng cc FAME trong dung dch nm
trong khong tuyn tnh kho st v tin hnh nh lng theo quy trnh.
Kt qu thc nghim thu c cho thy quy trnh phn tch c thu hi v ng
kh tt, sai s khi phn tch m c basa dao ng t -10,93% n 9,83%, m ln t -13,34%
n 9,70%, du u nnh t -10,64% n 9,79%, du m t -12,70% n 9,57%, du lc t -
11,95% n 9,81%, du da t -8,16% n 9,12%, du ht cao su t -10,29% n 8,87%, du
ht jatropha t -10,26% n 9,71%. Nh vy phng php nghin cu c sai s nm trong
ngng cho php, t -20% n 10% [22], p ng c yu cu phn tch.
3.3.4. Kim tra i chng kt qu phn tch
xem xt tnh chnh xc ca phng php nghin cu, chng ti tin hnh gi kim
nghim hm lng axit palmitic, axit oleic v axit linoleic trong mt mu m ng vt (m
c basa) v mt mu du thc vt (du m) n phng th nghim c cng nhn VILAS
(theo ISO 17025:2005) (h thng cng nhn phng th nghim ca Vit Nam), Vin Kim
nghim An ton V sinh thc phm Quc gia v so snh kt qu phn tch vi kt qu kim
nghim. Kt qu kim tra chnh xc ca phng php nghin cu c ch ra trn bng
3.28.
Bng 3.28. So snh kt qu phn tch v kt qu kim nghim mt s axit bo ca mu m c
basa v mu du m Vit Nam
Thng s
phn tch
Kt qu
phn tch
(mg/g)
Kt qu kim
nghim Vilas
(mg/g)
t
tn
(N=6)
M c basa
Axit
palmitic
227 238 2,570
Axit oleic 305 308 0,840
Axit linoleic 118 123 2,448
Du m
Axit
palmitic
77 79 2,330
Axit oleic 285 293 2,470
Axit linoleic 424 420 1,923
So snh kt qu phn tch vi kt qu kim nghim u thu c gi tr t
thc nghim
=
x . N / S (N = 6; S c tnh qua kt qu kho st lp li 6 ln hm lng cc FAME
trong mu m c basa v mu du m 3.3.2) b hn t
chun
(0,95; 5) = 2,571. Nh vy,
phng php xy dng t yu cu v ng [22].
Vy kt qu kim tra thng k cho thy phng php phn tch c lp li tt, nhy
v thu hi cao, t yu cu v chnh xc v tin cy, c th p dng trong vic phn
tch thnh phn axit bo trong cc mu DMTV Vit Nam.
3.4. Phn tch mu thc t
3.4.1. Chuyn i DMTV thnh FAME
p dng cc iu kin ti u tm c theo hai quy trnh chuyn i DMTV thnh
FAME dng metanol vi xc tc kim hoc axit c tin hnh 3.2. Vi cc mu m ln,
du u nnh, du m, du lc, du da s dng cc iu kin ti u ca quy trnh chuyn i
mt giai on xc tc kim nh mu m c basa. Vi du ht jatropha s dng cc iu kin
ti u ca phn ng este ha xc tc axit (giai on mt) ca quy trnh hai giai on iu ch
FAME nh du ht cao su.
Sau khi thc hin cc qu trnh chuyn i, chuyn i thnh FAME ca cc mu
DMTV c phn tch trn my UFLC v c tnh theo cng thc:
i i
i
S s
H% 100%
S

(3.11)
Trong :
i
s

: tng din tch pic ca cc triglyxerit cha chuyn i thnh FAME,

i
S

: tng din tch pic ca tt c cc triglyxerit ban u.

Kt qu chuyn i trung bnh ba ln o ca cc mu DMTV c th hin trn
bng 3.29.
Kt qu phn tch bng UFLC cho thy mc phn ng chuyn i este cc mu
DMTV nghin cu l rt cao (> 98%), hm lng monoglyxerit, diglyxerit v triglyxerit
sau phn ng ch l lng vt, qu trnh chuyn i c lp li tt, lch chun tng i
di 0,7%, sn phm thch hp tin hnh phn tch thnh phn FAME trn thit b
GC/FID.
Bng 3.29. chuyn i thnh FAME ca cc mu DMTV (n = 3)
DMTV
H
1

(%)
H
2

(%)
H
3

(%)
H
(%) SD
RSD
(%)
M c basa 99,3 100 99,9 99,7 1,0 0,4 0,38
M ln 100 99,9 99,8 99,9 0,2 0,1 0,10
Du u nnh 99,8 99,8 99,3 99,6 0,7 0,3 0,29
Du m 97,8 98,3 98,1 98,1 0,7 0,3 0,26
Du lc 99,1 98,1 97,9 98,4 1,5 0,6 0,65
Du Da 99,8 100 99,9 99,9 0,2 0,1 0,10
Du ht cao su 98,3 98,1 97,9 98,1 0,5 0,2 0,20
Du ht
jatropha
98,4 97,9 99,1 98,5 1,5 0,6 0,61
3.4.2. Xc nh axit bo trong cc mu DMTV Vit Nam
Sau khi chuyn i hon ton DMTV thnh FAME, t cc iu kin ti u tm c
ca phng php GC/FID tch v xc nh cc FAME chng ti p dng tch v xc nh
cc axit bo trong 8 mu DMTV Vit Nam. Kt qu phn tch thu c nh sau:
Trong m c basa c cha n 25 axit bo trong axit bo chim hm lng cao nht
l axit oleic (37%), tip n l axit palmitic (28%), axit linoleic (14%), axit stearic (8%), axit
myristic (5%), axit palmitoleic (1,4%), cc axit bo khc u c hm lng thp, di 1%.
Tng cc axit bo no (SFA) v axit bo khng no mt ni i (MUFA) gn xp x nhau,
tng ng l 43% v 38%, v gp khong 2 ln cc axit bo khng no nhiu ni i (PUFA)
(18%). Hm lng cc axit bo e-3 v e-6 trong m c basa l 155 mg trong 1g cht bo,
c bit trong c thnh phn ca DHA (5,52 mg/g) v EPA (1,53 mg/g) rt tt cho sc
khe.
Trong m ln c cha 15 axit bo v cng tng t nh trong m c basa, chim hm
lng ln nht l axit oleic (35%), tip n l axit palmitic (24%), axit linoleic (23%), axit
stearic (12%), cc axit bo khc u c hm lng thp. Tng cc SFA (38%) v MUFA
(37%) gn xp x 1,5 ln tng cc PUFA (25%). Hm lng cc axit bo e-3 l 7,6 mg/g cht
bo, chim gn 1% v hm lng cc axit bo e-6 l 193 mg/g cht bo, chim 24% trong
tng s cc axit bo. M ln ch yu cha cc axit bo mch ngn, khng thy s c mt ca
cc axit bo mch di C22 v EPA, DHA nh trong m c basa.
Trong du u nnh phn tch c 15 axit bo, trong tng hm lng cc MUFA
nhiu nht (39%), tip n l cc PUFA (32%) v thp nht l cc SFA (29%). Du u nnh
cha mt lng ng k cc axit bo e-3 (75 mg/g) v axit bo e-6 (188 mg/g).
Trong du m c cha 11 axit bo trong nhiu nht l PUFA, 51%, ch yu l axit
linoleic, tip n l MUFA, 34%, ch yu l axit oleic v ch c 15% cc SFA. Du m cng
cha lng ng k axit bo e-6 (424 mg/g) v c bit c cha lng b thnh phn ca
DHA (0,165 mg/g) m cc loi du thc vt khc khng c.
Trong du lc c cha 13 axit bo, nhiu nht l cc MUFA, 42%, ch yu l axit oleic,
tip n l cc PUFA, 35%, ch yu l axit linoleic v cha t hn cc SFA, 22%, ch yu l
axit palmitic. Du lc cng cha nhiu axit bo e-6 (288 mg/g) nhng lng axit bo e-3 th
rt t (0,66 mg/g).
i vi du da th khc vi cc du thc vt phn tch, thnh phn ch yu li l cc
SFA (8/12 axit bo), chim n 87%, nhiu nht l axit lauric (43%), axit myristoleic (19%),
axit palmitic (12%), v cha lng t cc MUFA (9%) v PUFA (3%). Duy nht ch c du
da l cha cc axit bo mch ngn C8, C10. Lng axit bo e-3, e-6 ca du da t hn rt
nhiu so vi cc du thc vt trn. Do du da ng rn iu kin thng v gi tr dinh
dng ca du da l thp nht.
Du ht cao su v du ht jatropha l hai loi du trong thnh phn c cha nhiu loi
c t v cc cht khng dinh dng (antinutritional) gy c hi i vi ngi v vt nui.
V vy hai loi du ny khng s dng lm thc n m ch yu nghin cu sn xut nhin
liu sinh hc, x phng v dc liu cho con ngi. Kt qu phn tch cho thy du ht cao
su v du ht jatropha c thnh phn gn tng ng nhau, gm 13 axit bo, trong nhiu
nht l cc PUFA (tng ng 46% v 43%), tip n l MUFA (34% v 35%) v cha t hn
cc SFA (19% v 21%), ch yu cng bao gm cc axit palmitic, stearic, oleic, linoleic.
Tm li, vi kt qu phn tch cc mu DMTV trn chng ti nhn thy: Du da cha
hm lng axit bo no cao nht, t axit bo khng no, nht l axit bo e-3, e-6 do t c gi
tr dinh dng nht, thch hp b sung vo thc n v lm ch phm dinh dng cho ng vt
nui. ch to nhin liu sinh hc t du da, cn c thm ph gia h nhit ng c v
nht cho nhin liu v nhin liu ny c hm lng axit bo no cao, nhit ng c,
nhit bt chy v nht cao, khng c li v mt kinh t.
Du m cha tng cc axit bo e-3, e-6 cao nht, gp khong 17 ln axit bo e-3, e-6
c trong du da v gp khong 2 ln axit bo e-3, e-6 c trong m c basa, m ln, du u
nnh, du lc v nht l thnh phn c cha DHA. Du u nnh th cha lng axit bo e-3
cao nht, do du m v du u nnh c gi tr dinh dng cao, thch hp s dng lm
thc n v thc phm dinh dng cho con ngi. Vi du lc, m ln v m c basa cng c
nhiu cc axit bo khng no, do c th s dng lm thc n cho ngi v ng vt nui.
Tuy nhin m c basa v m ln c cha nhiu axit bo no nn nu n nhiu s khng tt cho
sc khe. Do con ngi nn tng cng n cc loi du thc vt thay v thng xuyn s
dng cc loi m ng vt nh thi quen thng thng trc y.
M c basa, m ln c hm lng axit bo khng no thp hn du m, du u nnh,
du lc do biodiesel i t hai loi m ny s c ch s xetan cao hn v bn oxy ha tt
hn, ngc li nht v im ng c s cao hn biodiesel i t cc loi du thc vt trn.
Hai loi du khng n c l du ht cao su v du ht jatropha c hm lng axit bo
khng no cao hn rt nhiu axit bo no (gp khong 4 ln), nht, nhit ng rn v
nhit bt chy thp, c th ch to diesel sinh hc, nht l cc vng lnh. Tuy nhin v
c nhiu axit bo khng no nn nguyn liu cng d b oxy ha, polyme ha, phn hy nu
lu ngy, gy kh khn cho qu trnh bo qun, thi gian s dng ngn.
M c basa, m ln, du m, du u nnh, du lc va c th dng lm thc n, ch
phm dinh dng va c th s dng ch to biodiesel. Tuy nhin ngun nguyn liu ng,
thc vt Vit Nam hin nay ch yu dng trong thc phm vi sn lng thu hoch thp v
Nh nc cha c nh hng quy hoch nui trng lm nguyn liu cho cng nghip.
Trong nhng nm trc mt, nu khng c quy hoch vng nguyn liu cng nh cc chnh
sch h tr khc ca Nh nc th DMTV cha th coi l nguyn liu sn xut biodiesel
Vit Nam. Nguyn liu sn xut biodiesel c u th hn c l m c basa, m c tra, du m
thi hoc qua s dng. Du m thi hoc qua s dng gn nh thi b gy nhim mi
trng, ngun cung nh l, khng n nh. s dng lm nguyn liu sn xut biodiesel
cn phi thit lp h thng thu gom, tn tr v s ch m bo cung cp n nh cho sn xut.
Ngun nguyn liu t cy jatropha phi c mt chng trnh quc gia chuyn cy hoang ha
thnh cy cng nghip gn lin cc nhn t mi trng vi cng ngh sn xut du jatropha,
biodiesel v cc sn phm ph nh thc n gia sc, thuc tr su, dc phm,... M c basa
l sn phm ph c sn, r tin, sn lng tng nhanh trong nhng nm gn y do tnh hnh
xut khu phile c pht trin mnh, c bit l cc tnh ng bng sng Cu Long. V vy
khng nh hng n ngun lng thc, thc phm quc gia, ng thi tn dng c
ngun ph thi, hn ch gy nhim mi trng, li c nng sut thu hoch cao th dng ph
phm m c basa t cc nh my ch bin thy sn lm nguyn liu iu ch biodiesel l
thch hp hn c.


KT LUN

Trn c s cc kt qu nghin cu thu c, chng ti rt ra mt s kt lun sau:
1. Nhm xc nh chnh xc v chn lc ng thi 37 axit bo, s dng m hnh hi
quy bc hai tm trc giao xy dng phng trnh hi quy v nh gi nh hng ng thi
cc yu t n kh nng tch v xc nh cc axit bo trong du m ng, thc vt Vit Nam.
2. Trn c s d kin thc nghim ti u ha iu kin tch v xc nh ng thi 37
axit bo bng phng php sc k kh detector ion ha ngn la gm: Ct mao qun phn
cc mnh SP
TM
-2560 (100m 0,25mm 0,2m); chng trnh nhit : nhit u 140
0
C,
gi 5 pht, tng 2,4
0
C/pht ln 240
0
C, gi 8 pht; kh mang He, tc 20,5 cm/s; bm chia
dng t l 30:1.
3. thnh cng trong vic nghin cu mt cch c h thng kim tra hm lng axit
bo t do trong DMTV v chuyn i DMTV thnh FAME t kho st n l n m
hnh hi quy bc hai tm trc giao xt nh hng ng thi cc yu t n hiu sut chuyn
i thng qua phn mm Modde 5.0, bng phng php o hm xc nh cc iu kin ti
u ca phn ng, xy dng quy trnh chuyn i thch hp mt giai on xc tc kim v quy
trnh hai giai on, giai on u xc tc axit, giai on sau xc tc kim.
4. p dng quy trnh nghin cu chuyn i 8 mu DMTV thnh FAME, hiu sut
chuyn i trn 99%, lp li tt, lch chun tng i di 0,7%.
5. Kt qu phn tch hm lng cc axit bo c x l theo phng php thng k:
lch chun tng i ca hm lng cc FAME trong khong 0,87 5,18%; ng dao
ng t -13,34 9,83%; t yu cu v chnh xc v tin cy khi so snh kt qu phn
tch vi kt qu kim chng ca phng th nghim c cng nhn Vilas (ISO 17025:2005) -
Vin Kim nghim An ton V sinh Thc phm Quc gia.
6. tin hnh phn tch cc axit bo trong 8 mu DMTV Vit Nam: m c basa, m
ln, du u nnh, du m, du lc, du da, du ht cao su v du ht jatropha. Kt qu cho
thy du m v du u nnh c gi tr dinh dng nht, tip n l du lc, m c basa, m
ln, du da t c gi tr dinh dng. Du ht cao su v du ht jatropha c th s dng lm
nguyn liu chnh sn xut biodiesel.

KIN NGH
1. ngh s dng kt qu xy dng quy trnh phn tch v tin ti ph duyt thnh
phng php phn tch tiu chun xc nh thnh phn axit bo trong du m ng, thc vt.
2. p dng phng php xc nh axit bo nghin cu m rng cho nhiu i tng
du m ng, thc vt khc nhm cung cp thm s liu phc v cho cc nghin cu v dinh
dng, kim nghim thc phm, dc liu, thc n gia sc, nhin liu sinh hc,



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