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TN LONG DY
Cn Th, 6/2013
I HC CN TH
KHOA KHOA HC T NHIN
B MN HA HC
--------
TN LONG DY
LUN VN TT NGHIP I HC
Ngnh: Ha hc
MSSV: 2096740
Cn Th, 6/2013
TRNG I HC CN TH
KHOA KHOA HC T NHIN
Nm hc 2012-2013
ti:
LY TRCH V KHO ST THNH PHN HA HC
CA TINH DU BC H (MENTHA ARVENSIS L.)
LI CAM OAN
......................................................................................................................................
......................................................................................................................................
......................................................................................................................................
......................................................................................................................................
Cn Th, ngy
thng
nm 2013
bo v v c duyt
Hiu trng..
Trng khoa..
Trng b mn
Cn b hng dn
c lp T do Hnh phc
B MN HA HC
MSSV: 2096740
Lp: C nhn Ha hc
Kha: K35
6. Mc tiu ca ti:
+ Kho st iu kin ti u khi ly trch tinh du Bc h bng phng
php chng ct li cun hi nc .
+ Xc nh cc ch s ha l ca tinh du Bc h.
+ Xc nh thnh phn tinh du Bc h bng GC MS
7. Cc ni dung chnh: ti gm cc phn
+ Phn 1: Tng quan
+ Phn 2: Thc nghim
+ Phn 3: Kt qu v tho lun
ii
Tn Long Dy
KIN CA B MN
....
CN B HNG DN
KIN CA HI NG LV V TLTN
iii
c lp T do Hnh phc
B MN HA HC
NHN XT V NH GI CA CN B HNG DN
1. Cn b hng dn: TS. Nguyn Trng Tun v ThS. Phm Quc Nhin
2. Tn ti: Ly trch v kho st thnh phn ha hc ca tinh du Bc h (Mentha
arvensis L.)
3. Sinh vin thc hin: Tn Long Dy
MSSV: 2096740
Lp C nhn Ha hc
4. Ni dung nhn xt:
a. Nhn xt v hnh thc ca lun vn tt nghip:..........................................
..................................................................................................................................
..................................................................................................................................
b. Nhn xt v ni dung ca lun vn tt nghip ( ngh ghi chi tit v y
): ............................................................................................................
..................................................................................................................................
..................................................................................................................................
Nhng vn cn hn ch: ..................................................................
..................................................................................................................................
..................................................................................................................................
c. Nhn xt i vi sinh vin thc hin ti: ...............................................
..................................................................................................................................
..................................................................................................................................
d. ngh v im: .......................................................................................
..................................................................................................................................
..................................................................................................................................
Cn th, ngy
thng nm 2013
Cn b hng dn
iv
c lp T do Hnh phc
B MN HA HC
MSSV: 2096740
Lp C nhn Ha hc
4. Ni dung nhn xt:
a. Nhn xt v hnh thc ca lun vn tt nghip: .........................................
..................................................................................................................................
..................................................................................................................................
b. Nhn xt v ni dung ca lun vn tt nghip ( ngh ghi chi tit v y
): .................................................................................................................
..................................................................................................................................
Nhng vn cn hn ch: ..................................................................
..................................................................................................................................
..................................................................................................................................
c. Nhn xt i vi sinh vin thc hin ti: ...............................................
..................................................................................................................................
..................................................................................................................................
d. ngh v im: .......................................................................................
..................................................................................................................................
..................................................................................................................................
Cn th, ngy
thng
nm 2013
Cn b phn bin
LI CM N
LI CM N
-----------c ngi trn ging ng ca trng i hc Cn Th hc tp trong sut bn
nm qua l nim vinh d i vi em. Tng bui hc, tng bi ging, tng kinh nghim
m cc thy, cc c truyn t li lun l ngun kin thc qu bu cho em. Nhng
kin thc y gi y tr thnh kinh nghim v cng qu gi gip em thc hin tt
lun vn tt nghip, cng nh l nn tng vng chc cho em bc i nhng bc trn
ng i sau ny. Em xin gi li cm n su sc n:
TS. Nguyn Trng Tun v ThS. Phm Quc Nhin lun quan tm hng dn
v to mi iu kin thun li em c th hon thnh tt lun vn ca mnh.
Qu Thy C ca trng i hc Cn Th, nhng ngi truyn t cho em
nhng kin thc qu bu v b ch lm hnh trang vo i.
Qu Thy C B mn Ha hc v B mn Sinh hc Khoa Khoa hc T nhin,
trng i hc Cn Th to mi iu kin v tn tnh gip em hon thnh tt
lun vn.
C s ging cy trng Bnh Chu (24, in Bin Ph, qun Bnh Tn, TP HCM)
nhit tnh gip em c c ngun nguyn liu tt nht em hon thnh qu
trnh thc nghim.
Cm n cc anh ch v cc bn phng th nghim Ha sinh gip v cho li
khuyn qu bu trong qu trnh em thc hin lun vn.
c bit em xin gi li cm n n gia nh, ngi thn v cc bn trong lp C
nhn Ha K35. Nhng ngi lun bn em, ng vin, ng h v gip em c v
vt cht ln tinh thn em c th hon thnh tt lun vn ca mnh.
Em xin chn thnh cm n tt c mi ngi!
Cn th, ngy
thng
K tn
nm 2013
Tn Long Dy
vi
MC LC
MC LC
-----------LI CAM OAN.........................................................................................................i
PHIU NG K TI LUN VN TT NGHIP............................................ii
NHN XT V NH GI CA CN B HNG DN....................................iv
NHN XT V NH GI CA CN B PHN BIN........................................v
LI CM N ............................................................................................................vi
MC LC.................................................................................................................vii
PH LC HNH ........................................................................................................ix
PH LC BNG........................................................................................................x
DANH SCH CC T VIT TT ...........................................................................xi
LI M U ...........................................................................................................xii
CHNG I .................................................................................................................1
Tng quan...................................................................................................................1
I.1 GII THIU H LAMIACEAE .......................................................................1
I.1.1 Phn loi hc[1,2]..........................................................................................2
I.1.2 M t[1,2] .....................................................................................................3
I.1.3 Phn b v thu hi[1,2] ..................................................................................3
I.1.4 Cng dng ca Bc h ................................................................................4
I.2 TINH DU........................................................................................................5
I.2.1 Khi qut v tinh du ..................................................................................5
I.2.2 Qu trnh tch ly[3,4,5] .................................................................................5
I.2.3 Tinh du Bc h[3] .....................................................................................6
I.3 TNH HNH NGHIN CU TINH DU BC H ..........................................7
I.3.1 Kho st hot tnh khng vi sinh vt ca tinh du Bc h Mentha
piperita L. [13] ......................................................................................................7
I.3.2 Thnh phn tinh du ca Bc h Mentha arvensis L. v Bc h Mentha
piperita L. nhng giai on sinh trng khc nhau trong vng Kumaon thuc
pha ty Himalaya. ...............................................................................................9
I.3.3 Tch v tng hp menthol..........................................................................12
I.4 MT S PHNG PHP LY TRCH TINH DU BC H........................12
I.4.1 Phng php c hc[5,6] .............................................................................13
I.4.2 Phng php dng dung mi ha tan[5,6] ...................................................13
I.4.3 Phng php chng ct li cun hi nc[4,5,6] ..........................................14
I.4.4 Phng php chit Soxhlet[5].....................................................................15
CHNG II: THC NGHIM.................................................................................16
II.1 A IM, THI GIAN, THIT B, NGUYN LIU V HA CHT ......16
II.1.1 a im v thi gian ..............................................................................16
II.1.2 Thit b, nguyn liu, dng c v ha cht ...............................................16
II.2 PHNG PHP NGHIN CU...................................................................17
II.2.1 X l nguyn liu ....................................................................................18
II.2.2 Ly trch tinh du bng phng php li cun hi nc[7] .........................18
II.2.3 Xc nh mt s ch tiu ha l ca tinh du Bc h .............................19
vii
MC LC
viii
PH LC HNH
PH LC HNH
-----------Hnh 1: V tr trong phn loi thc vt ca Bc h Mentha arvensis L..........................2
Hnh 2: L v cy Mentha arvensis L. .........................................................................3
Hnh 3: Thn v hoa Mentha arvensis L. .....................................................................3
Hnh 4: Tinh du Bc h ..............................................................................................6
Hnh 5: H thng Soxhlet ..........................................................................................12
Hnh 6: Mu Bc h kh ............................................................................................17
Hnh 7: Mu Bc h ct nh .................................................................................17
Hnh 8: S cc bc thc hin ly trch tinh du Bc h bng phng php chng
ct li cun hi nc .................................................................................................19
Hnh 9: Chng trnh nhit ca GC - MS chy phn tch thnh phn ha hc tinh
du Bc h .................................................................................................................24
Hnh 10: iu kin chy ca MS ...............................................................................24
Hnh 11: iu kin Injecter........................................................................................25
Hnh 12: Tinh du bc h..........................................................................................26
Hnh 13: th biu din thi gian ly trch theo hm lng tinh du Bc h thu
c ..........................................................................................................................28
Hnh 14: th biu din nhit ly trch theo hm lng tinh du Bc h thu c 30
Hnh 15: th biu din th tch dung mi ly trch theo hm lng tinh du Bc h
thu c ....................................................................................................................31
Hnh 16: Cng thc ca mt s thnh phn chnh trong tinh du Bc h....................34
Hnh 17: Ph phn tch thnh phn tinh du Bc h bng GC - MS.......................34
Hnh 18: Khi ph ca menthol .................................................................................35
Hnh 19: Khi ph ca menthol cung cp t th vin ph NIST ...............................35
Hnh 20: S phn mnh ca phn t menthol ........................................................36
ix
PH LC BNG
PH LC BNG
-----------Bng 1: Cc ch s l ha ca tinh du Bc h ..........................................................6
Bng 2: Thnh phn ha hc chnh ca tinh du Mentha piperita L. xc nh bng
phng php GC MS. ...............................................................................................8
Bng 3: Kt qu hot tnh khng khun (MIC, mg/ml).................................................8
Bng 4: Thnh phn ha hc ca Bc h Mentha arvensis L.[15] ................................10
Bng 5: Thnh phn ha hc ca Bc h Mentha piperita L.[15] .................................11
Bng 6: Kt qu chun xc nh ch s acid ..........................................................26
Bng 7: Kt qu chun xc nh ch s savon v ch s ester.................................27
Bng 8: Kt qu kho st thi gian ly trch tinh du bc h bng phng php chng
ct li cun hi nc .................................................................................................28
Bng 9: Kt qu kho st nhit ly trch tinh du bc h bng phng php chng ct
li cun hi nc.......................................................................................................29
Bng 10: Kt qu kho st th tch dung mi ly trch tinh du bc h bng phng
php chng ct li cun hi nc ..............................................................................30
Bng 11: Bng so snh thnh phn ha hc ca 4 mu TIME TU, VOL TU, TEM
TU v MAU KS tinh du bc h bng phng php chng ct li cun hi nc 32
Bng 12: Thnh phn chnh trong tinh du Bc h.....................................................36
Bng 13: So snh kt qu nghin cu thnh phn Bc h Mentha arvensis L. Vit Nam
v Mentha arvensis L. Himalaya................................................................................37
Bng 14: Kt qu iu kin ti u cho qu trnh ly trch ...........................................39
Bng 15: Cc ch s ha hc ca tinh du Bc h ......................................................39
PH LC BNG
GC MS
IA
Acid index
IS
Savon index
IE
Ester index
FID
MIC
APG III
xi
LI M U
LI M U
-----------Trc chin tranh th gii th nht, Nht Bn c xem l nc dn u trong
sn sut cc sn phm thng mi t cy Bc h nh: dc phm, kem nh rng,
nc xc ming, ko thuc l, m phm, trn th trng th gii. Thi gian ny
c xem l thi k thnh vng ca cy Bc h Mentha arvensis Nht Bn v n
cn c gi l Japani mint. Sau chin tranh th gii th hai, Nht Bn chuyn sang
trng cy Bc h phc thng mi v xut khu sang Brazin v Bc M. Cng thi
gian ny, n , Trung Quc, M, v nhiu nc khc cng c nhng thnh tu ni
bt trong sn sut cc sn phm t Bc h. Nm 1960, n l nc sn sut tinh du
Bc h ln nht th gii. Trung Quc lc ny cng c xem l ngun cung cp
menthol chnh cho th trng thi gii.
Bn cnh nhng gi tr kinh t mang li, th Bc h cn c mt vai tr quan trng
trong ng Y l cha tr cc bnh nh cm st, au nhc bn chn, vt cn trng
cn[1], Nhng a phn Bc h dng cha tr l s dng hn hp ton phn hoc
theo kinh nghim dn gian. V th vic nghin cu thnh phn ha hc cy Bc h
tm nhng hp cht c cu trc mi hoc nhng cht c tc dng chnh s dng
di dng tinh khit cng nh trong iu tr bnh l vic lm cn thit.
Chnh v cy Bc h c nhiu cng dng nh vy nn rt sm c nhiu cng
trnh nghin cu v cy ny nhng a s l ngoi nc. Nhm gp phn lm r hn
thnh phn ha hc ca cy Bc h, nn em chn ti Ly trch v kho st thnh
phn ha hc ca tinh du Bc h (Mentha arvensis L.) gp phn gip cho vic
bo ch v s dng c thun li hn. ng thi nng cao gi tr s dng ca cy
Bc h. Trong gii hn nghin cu ca ti em tin hnh nghin cu mt s vn
sau:
Nghin cu iu kin ly trch ti u ca tinh du Bc h bng phng php
chng ct li cun hi nc.
Xc nh cc ch tiu ha l ca tinh du Bc h.
Xc nh thnh phn ha hc chnh trong tinh du Bc h bng phng php
GC MS.
xii
CHNG I
TNG QUAN
(Ngun: http://blog.daum.net)
Bc h (Mentha arvensis L.) l mt loi cy tho sng lu nm. Thn mm, hnh
vung. Loi thn ngm mang r mc b lan, loi thn ng mang l, cao t 0,300,40m, c th cao ti 1m, mu xanh lc hoc tm ta, i khi phn nhnh. L mc
i, cun ngn, phin l hnh trng hoc hnh bu dc, mp c kha rng u, mt
trn v mt di u c lng che ch v lng bi tit.
Hoa mc vng k l, cnh hoa hnh mi mu tm hay hng nht c khi mu
trng, trng c ng ngn, phin trng chia lm bn phn bng nhau, c mt vng lng
pha trong. Bn nh bng nhau ch nh nhn. t khi thy c qu v ht.
Ton thn c lng che ch v lng tit tinh du v c mi thm. Ma hoa qu
vo thng 7-10.
I.1.3 Phn b v thu hi[1,2]
Cy Bc h nc ta thng mc hoang, v mt s c trng ly l v cy
lm thuc. Gn y, Bc h c trng nhiu ly tinh du nh lng Ngha
I.2 TINH DU
I.2.1 Khi qut v tinh du
Tinh du l mt hn hp nhiu cht d bay hi, c mi c trng ty thuc vo
ngun gc nguyn liu cung cp tinh du. Phn ln tinh du c ngun gc t thc vt
v s t t ng vt. Trong thin nhin tinh du trng thi t do, ch c mt s t
trng thi tim tng, ngha l tinh du khng c sn trong nguyn liu m ch xut hin
trong nhng iu kin gia cng nht nh trc khi tin hnh ly trch hay di tc
dng c hc. Cn trng thi t do, tinh du c sn trong nguyn liu c th thu hi ly
trch trong iu kin bnh thng[3].
I.2.2 Qu trnh tch ly[3,4,5]
Trong thc vt tinh du c to ra v tch ly trong cc m. Hnh dng cc m
ny thay i ty theo v tr ca chng trong cy. Nhng m ny c th hin din tt
c cc b phn ca cy nh r, thn, l, hoa v c trivi nhng tn gi khc nhau
nh:
T bo tit: tinh du c tit ra ri chng c gi trong t bo (m tit) v d
trong cnh hoa hng, trong c gng
Lng tit: cng l t bo tit nhng nm nh ra ngoi thc vt, thng bt gp
cc loi hoa mi, cc, c
Ti tit: t bo tit ra tinh du nhng khng cha li bn trong m dn chung
cha vo mt xoan trng, to ra bi c ch ly bo hay tiu bo. Ti tit thng nm
bn di lp biu b. Thng c cc ging Cirtrus, eucalyptus
ng tit: cch to ra tinh du cng ging nh ti tit nhng nm su trong phn
g v chy di theo s g, thng bt gp trong cc ging Dipterocarpi, Artemisia
Hnh 4: Tinh du Bc h
(Ngun: http://tinhdauthomtv.com)
L mt cht lng c mu vng nht, mi Bc h, thanh mt v c v t. Thu c
bng cch chng ct li cun hi nc l Bc h.
Thnh phn, tnh cht ca tinh du Bc h ty thuc vo ging, t ai, kh
hu... Trn th gii hin nay c cc ging Bc h chnh nh sau: Nga, Anh, M,
Php, Trung Quc v Nht Bn. Loi tinh du Bc h tt nht hin nay l t Bc h
Nht Bn (Mentha arvensis L.).
Cc ch s l ha ca tinh du Bc h Mentha arvensis L. nh sau:
Bng 1: Cc ch s l ha ca tinh du Bc h
Thng s
d 20
n 20
D
[]D
IA
IS
IE
Gi tr
0,895
1,4580
-24o
11
Trong :
d 20
: t trng ca tinh du Bc h.
n 20
D
[]D
: quay cc ca tinh du Bc h.
IA
: ch s acid ca tinh du Bc h.
IS
: ch s ester ca tinh du Bc h.
Limonene
1,9
1,3
1,0
2,1
1,8-Cineole
5,3
4,0
3,4
4,0
Menthone
27,9
21,2
27,2
18,4
Menthofuran
5,5
3,8
1,3
3,2
Isomenthone
3,5
2,9
3,8
2,9
Linalool
2,5
4,4
4,1
4,8
-Caryophyllene
4,2
1,8
1,6
1,5
Terpinen-4-ol
1,2
3,4
3,8
2,1
Menthol
27,5
42,3
39,9
34,6
Pulegone
6,4
1.0
1,9
14,4
-Terpineol
2,4
1,6
1,7
0,7
M1
M2
Escherichia coli
2,5
1,25
1,25
1,25
1,25
5,0
Staphylococcus aureus
0,625
0,625
1,25
2,5
0,625
2,5
Pseudomonas aeruginosa
2,5
2,5
5,0
2,5
2,5
5,0
Enterobacter aerogenes
1,25
1,25
1,25
2,5
1,25
5,0
Proteus vulgaris
2,5
5,0
1,25
1,25
1,25
2,5
Salmonella typhimurium
1,25
1,25
1,25
2,5
0,625
5,0
Klebsiella pneumoniae
2,5
2,5
2,5
2,5
2,5
5,0
Yersinia enterocolitica
2,5
2,5
2,5
2,5
2,5
2,5
Listeria monocytogenes
0,156
0,625
2,5
0,312
0,625
1,25
Bacillus cereus
1,25
1,25
1,25
1,25
1,25
1,25
0,625
2,5
0,625
1,25
0,625
0,625
Staphylococcus
epidermidis
0,625
0,312
0,625
0,156
0,625
2,5
2,5
1,25
1,25
0,625
1,25
2,5
0,07
0,07
0,625
0,312
0,07
1,25
0,312
0,156
0,312
0,312
0,156
2,5
0,156
0,156
0,312
0,156
0,156
1,25
0,625
0,625
0,312
0,625
0,625
2,5
Trong :
M1 : (-)-menthol
M2 : (-)-menthone
I.3.2 Thnh phn tinh du ca Bc h Mentha arvensis L. v Bc h
Mentha piperita L. nhng giai on sinh trng khc nhau trong vng
Kumaon thuc pha ty Himalaya.
Th nghim c tin hnh kho st trn hai loi ging: Bc h Mentha arvensis L.
cc khu vc Kosi, Saksham, Alka v Himalaya; loi th hai l Bc h Mentha
piperita L. trng khu vc Kukrail, CIM-Madhurus v CIM-Indus. Ging Bc h
Mentha arvensis L. c trng vo thng ba v ging Bc h Mentha piperita L.
c trng vo thng ging. Cc ging c thu hi sau khi c 90 ngy tui (tnh
t lc bt u gieo trng). Tin hnh ly trch tinh du trn mu ti sau khi c
thu hi bng phng php chng ct li cun hi nc.
Sau tinh du ca hai ging Bc h thu c s c phn tch thnh phn
ha hc bng phng php sc k kh s dng u d FID. Ct s dng l ct mao
qun silica (30 m x 0.25 mm x 0.25 m), pha tnh l BP-20, kh mang s dng l
kh hidro. Kt qu thnh phn tinh du thu c nh sau:
Kosi
Saksham Himalaya
-Pinene
0,47
0,61
0,55
1,25
-Pinene
0,56
0,79
0,24
0,86
Sabinene
0,14
-Myrcene
0,40
0,40
0,31
0,49
-terpinene
Limonene
1,57
0,98
0,67
1,85
1,8- cineole
0,11
-terpinene
(E)- -ocimene
(Z)-3-hexanol
3-octanol
1,61
4,24
1,73
Menthone
7,46
6,53
5,08
11,85
(E)-sabinene hydrate
Iso-menthone
3,56
3,48
3,16
6,09
Linalool
Menthyl acetate
1,12
1,44
1,63
3,67
Isopulegol
1.01
0,94
0,73
1,16
-Caryophyllene
Neo-menthol
1,93
1,74
1,61
1,45
Terpinen-4-ol
0,65
0,33
0,31
0,40
Pulegone
0,34
Menthol
77,54
75,85
79,64
65,61
Isomenthhol
0,15
0,11
-terpineol
0,17
0,17
0,18
Germacrene D
0,16
0,14
0,31
Piperitone
0,24
1,76
1,08
2,05
Cavone
10
Kalka
Kukrail
CIM-Madhurus
CIM-Indus
-Pinene
0,91
1,00
0,88
-Pinene
0,55
1,48
Sabinene
0,22
1,64
-Myrcene
0,24
0,26
0,42
-terpinene
0,21
0,18
15,46
Limonene
2,37
1,54
0,51
1,8- cineole
5,58
6,57
5,96
-terpinene
0,55
0,35
13,94
(E)- -ocimene
0,30
1,29
3,65
p-cimene
0,37
0,18
1,38
3-octanol
0,43
Menthone
29,83
26,88
0,77
Menthofurane
0,81
0,32
7,45
Iso-menthone
3,36
2,65
1,37
Linalool
0,19
0,26
0,34
Menthyl acetate
5,18
7,23
1,23
Isopulegol
0,13
0,13
0,27
-Caryophyllene
0,96
1,10
4,13
Neo-menthol
3,47
3,39
0,38
Terpinen-4-ol
0,51
1,21
2,07
Pulegone
0,68
0,96
Menthol
37,44
36,13
22,56
(E)- -farnesene
0,18
0,21
0,40
Isomenthhol
0,19
0,25
-terpineol
0,16
0,16
0,44
11
0,78
0,69
2,49
Piperitone
1,27
0,83
1,19
Cavone
0,52
12
13
15
16
Hnh 6: Mu Bc h kh
Hnh 7: Mu Bc h ct nh
Nc ct
Phenolphthalein (5 ml)
bt (5 g)
Diethyl eter
18
Nguyn liu
+ Loi b c, l cy tp
+ Ct nh
Ly trch bng li
cun hi nc
Hn hp tinh du
+ Chit hn hp vi diethyl
ether loi b tp cht
Nc
Dung mi
+ Chit li hn hp vi
diethyl ether
Nc
Dung mi
Tinh du bc h
th
19
5,61 V
m
Trong :
5,61 l lng miligam KOH cha trong 1 ml KOH 0,1N.
V : th tch ml KOH 0,1N dng chun mu th nghim.
m: lng tinh du dng th nghim (g).
II.2.3.3 Xc nh ch s savon ha[3,6,7]
Ch s x phng l s miligam KOH cn thit trung ha tt c cc acid t do
v acid kt hp c trong 1 gam tinh du.
Cch xc nh
Cn chnh xc khong 0,3 gam tinh du vo bnh tam gic 250 mL, cho vo
6 mL KOH 0,1 N trong alcol. Tin hnh song song vi mu khng c du. em 2 bnh
un cch thy qua ng sinh hn, cho si nh trong khong 45 pht tinh du thy
phn hon ton. ngui, thm vo 2 mL nc ct, 2-3 git phenolphthalein, dung
dch chuyn sang mu hng, chun bng HCl 0,1 N trong alcol cho n khi mt
mu hng.
Tin hnh chun mu trng trc khi chun mu tht.
Tnh kt qu: I S =
5,61 (V1 V2 )
m
Trong :
1mL KOH 0,1 N tng ng vi 5,61 mg KOH
IS: Ch s x phng
V1 : s mL HCl 0,1N dng chun bnh khng
V2 : s mL HCl 0,1N dng chun bnh cha mu
21
23
24
25
Ln 1
Ln 2
Ln 3
Trung bnh
1,0030
1,0032
1,0042
1,0035
0,3200
0,3200
0.3000
0,3133
IA
1,75
26
Khi lng
tinh du (g)
Ln 1
Ln 2
Ln 3
Trung bnh
1,0034
1,0030
1,0030
1,0031
17,6
17,5
17,4
17,5
14,6
14,7
14,5
14,6
Th tch HCl
0,1 N chun
mu (ml)
Th tch HCl
0,1 N chun
mu trng (ml)
IS
16,22
IE
14,47
III.2
27
Khi
lng
mu (g)
Khi lng
tinh du (g)
Hm
lng %
tinh du
30
0,2066
1,033
40
0,3146
1,573
0,3770
1,885
60
0,4715
2,358
75
0,3755
1,878
90
0,3746
1,873
50
20
Dung mi
Nc ct
Th tch
dung mi
(ml)
500
Nhit
oC
120
30
40
50
60
70
80
90
100
Pht
Hnh 13: th biu din thi gian ly trch theo hm lng tinh du Bc h
thu c
Nhn xt: Qua qu trnh kho st v phn tch s liu thu c, cho thy rng: khi
thi gian ly trch tng th hm lng phn trm theo khi lng ca tinh du ly trch
cng tng. V nu thi gian ly trch lu hn 60 pht, nhn thy rng hm lng tinh
du gim li. Nh vy hm lng tinh du t cao nht l 2,358% thi gian 60 pht.
28
60
Khi
lng
mu (g)
20
Dung
mi
Nc ct
Th tch
dung
mi (ml)
500
Nhit
oC
Khi lng
Hm lng
tinh du
% tinh du
(g)
110
0,2991
1,4955
120
0,3082
1,541
130
0,3602
1,801
140
0,3277
1,6385
150
0,2629
1,3145
160
0,2601
1,3005
29
110
120
130
140
150
160
170
nhit
Hnh 14: th biu din nhit ly trch theo hm lng tinh du Bc h thu
c
Nhn xt: th trn cho thy rng: hm lng phn trm theo khi lng ca
tinh du ly trch tng khi tng nhit ly trch v hm lng t cao nht l 1,801%
nhit l 130 oC. Nhn thy rng nu tip tc tng nhit cao hn na th hm
lng tinh du t l nghch vi nhit . Cho nn em chn nhit ny lm nhit
ti u v c nh nhit 130 oC cho kho st tip theo.
III.2.3 Kho st lng dung mi ly trch
Tin hnh kho st ly trch 20 g mu Bc h kh vi nhng th tch nc ct khc
nhau thu c kt qu nh sau:
Bng 10: Kt qu kho st th tch dung mi ly trch tinh du bc h bng
phng php chng ct li cun hi nc
Thi
gian ly
trch
(pht)
60
Khi
lng
mu (g)
Dung
mi
20
Nc ct
Th tch
dung mi
(ml)
Khi lng
tinh du
(g)
Hm lng
% tinh du
0,2095
1,0475
300
0,3300
1,6500
400
0,3618
1,8090
500
0,2986
1,4930
200
30
Nhit
oC
130
0,2748
1,3740
700
0,2664
1,3320
ml
0,0
100
200
300
400
500
600
700
800
Hnh 15: th biu din th tch dung mi ly trch theo hm lng tinh du
Bc h thu c
Nhn xt: th cho thy khi tng th tch nc ct dng ly trch tinh du th
hm lng phn trm tinh du tng t l thun. V th tch nc ti a thu c
hm lng tinh du cao nht 1,809% l 400 ml. Nu thm nc tip tc nhn thy rng
hm lng tinh du khng tng na m gim li. Cho nn em chn th tch ny lm
th tch ti u.
III.1.4 Kho st s nh hng ca thi gian, nhit v th tch dung
mi n thnh phn ha hc tinh du Bc h
Tin hnh phn tch thnh phn ha hc ca 4 mu: mu kho st thi gian ti u
M1, mu kho st nhit ti u M2, mu kho st th tch ti u M3, mu kho st
c ba iu kin ti u M4. Thu c kt qu so snh nh sau:
31
Thi
gian lu
Thnh phn ha hc
2,29
M1
M2
M3
M4
-Pinene
0,02
0,62
0,53
2,86
-Pinene
0,04
1,05
0,97
3,08
-Myrcene
0,29
0,24
3,21
3-Octanol
0,04
0,05
0,69
0,68
3,7
Limonene
0,1
0,14
1,7
1,55
5,13
-Linalool
0,09
0,14
6,08
Isopulegol
0,2
0,25
1,25
1,21
6,25
trans-Menthone
9,32
9,43
14,37
16,23
6,76
(-)-Menthol
52,05
47,01
53,77
55,17
7,14
-Terpineol
0,09
8,04
3,4,4-Trimethyl-5-oxo2-hexenoic acid
0,06
8,27
Pulegone
0,2
0,24
7,36
7,15
8,63
Piperitone (p-Menth-1en-3-one)
7,99
9,38
2,53
2,26
9,62
Menthyl acetate
18,37
18,17
1,83
1,45
11,7
-Bourbonene
0,06
12,29
Longifolene
0,03
12,47
-Caryophyllene
1,16
1,67
13,59
Germacrene D
0,16
0,26
14
4-Chloro-2,3dimethyl-1,3hexadiene
0,26
0,53
15,11
(-)-Calamenene
0,17
0,2
15,42
-Muurolene
0,03
16,39
Caryophyllene oxide
0,07
17,14
-Cedrene
0,1
17,92
-Cadinol
0,05
32
0,1
0,49
0,03
0,74
0,28
0,27
0,06
0,02
0,11
0,03
(-)-
33
(-)-Menthol
Trans-Menthone
Pulegone
Menthyl
acetate
-caryophyllene
34
100
81
95
HO
50
55
41
69
123
43
56
27
15 18
138
39
31
109
53
36
45 48 51
10
20
30
40
50
(mainlib) Cyclohexanol, 5-methyl-2-(1-methylethyl)-, (1,2,5)-
10 largest peaks:
71 999 | 81 712 | 95 689 |
82 357 | 69 302 | 123 276 |
55 405 |
96 261 |
61 65
60
73
70
97
79
80
90
105
100
112
110
141
119
120
130
140
41 383 |
67 254 |
35
155
150
160
170
Thi gian lu
(pht)
2,29
2,86
3,08
3,21
3,7
5,13
6,08
6,25
6,76
8,27
8,63
-Pinene
-Pinene
-Myrcene
3-Octanol
Limonene
-Linalool
Isopulegone
trans-Menthone
(-)-Menthol
Pulegone
Piperitone
36
Menthyl acetate
-Caryophyllene
Germacrene D
1,45
0,28
0,27
Nghin cu
Trong nc[16]
Nc ngoi [15]
0,53
0,97
0,24
0,68
1,55
0,1
1,21
16,23
55,17
7,15
2,26
1,45
0,28
0,27
1,10
1,11
0,18
0,45
2,87
19,82
51,87
1,13
6,28
2,53
0,60
0,67
0,55
0,25
0,31
0,67
5,08
79,64
0,73
1,08
1,63
-
38
Thi gian
Th tch dung
(pht)
mi (ml)
60
400
Nhit oC
130
Hm lng
cao nht %
1,8
Xc nh c ch s ha hc ca tinh du Bc h nh sau:
Bng 15: Cc ch s ha hc ca tinh du Bc h
Ch s
IA
IS
IE
Gi tr
1,75
16,22
14,47
40
PH LC PH GC MS
PH GC MS CA TINH DU BC H LY TRCH THI GIAN TI U
(M1)
(-)-Menthol
Menthyl
acetate
Trans-Menthone
Piperitone
-caryophyllene
(-)-Menthol
Trans-Menthone
Pulegone
Piperitone
-caryophyllene
(-)-Menthol
Menthyl
acetate
Trans-Menthone
Piperitone
-caryophyllene
(-)-Menthol
Trans-Menthone
Pulegone
Menthyl
acetate