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XC NH CC NGUYN T VI LNG TRONG CM HOA OI HNG

(Lavandula angustifolia Mill.) H thng du hoa oi hng


Tc gi : Stanislav Bozhanov, Irina Karadjova, Stoyan Alexandrov.
Nhn : 09/12/2006
Nhn vi bn sa i: 13/01/2001
Chp nhn : 15/01/2007
ng trc tuyn: 23/01/2007

TM LC
Bulgaria l mt nh sn xut tinh du ni ting th gii. Kim sot cht lng sn xut
cc loi du hoa oi hng l mt cng vic phn tch quan trng bi v chng c s
dng rng ri trong qu trnh ch bin nc hoa v m phm, trong ngnh cng nghip
thc phm v hng liu. Nhng Bi vit gn y nghin cu v mi quan h gia cc
nguyn t vi lng cha trong cm hoa oi hng (Lavandula angustifolia Mill.) v trong
du hoa oi hng c ngun gc t hoa ny. Ba khu vc kiu mu c nghin cu
cn k: hai trong s c t xa cc khu cng nghip lng Zelenikovo v th trn
Pavel Banya, v mt khu vc c t gn nh my luyn kim loi mu Plovdiv. Cc
nguyn t Cd, Cr, Cu, Fe, Mn v Pb cha trong thc vt c xc nh sau khi acid
ha bi ngn la v nhit in quang ph hp th nguyn t (ETAAS). Cc loi
du hoa oi hng c phn tch ngay bng phng php ETAAS. Cc kt qu r rng
ch cho thy rng khng c s tng quan bn vng gia cc nguyn t vi lng cha
trong cm hoa v tinh du. C th gi nh rng cc nguyn t vi lng hin din v tch
ly trong cm hoa khng chuyn qua tinh du hoa oi hng trong sut qu trnh sn xut
bng cch chng ct hi nc.
2007 Elsevier B.V. Tt c cc quyn.
T kha: du hoa oi hng; cm hoa oi hng; AAS(pp o ph hp th nguyn t); cc
nguyn t vi lng; s tng quan.
1. GII THIU
Du hoa oi hng cht lng cao c sn xut thng qua chng ct hi nc t cm
hoa oi hng (Lavandula angustifolia Mill.). Mt kg du hoa oi hng c ly t
khong 120-150kg cm hoa oi hng, ty thuc vo iu kin kh hu. Tinh du hoa oi
hng l cc th m rt phc tp gm c nhiu lp khc nhau ca cc hp cht hu c
terpenes, hydrocarbons, esters, alcohols, aldehydes, ketones, vn vn. [1,2]. Tinh du
c s dng rng ri trong nc hoa v m phm v trong ngnh cng nghip thc
phm [3-5]. Tnh nng cha bnh v st khun ca chng cng c bit n nhiu [5-9].
Vic s dng rng ri tinh du i hi s kim sot nghim ngt i vi nhng tp cht
khng mong mun khc nhau, chng hn nh thm vo cc hp cht nhn to [10,11], d
lng thuc tr su [12,13], cc yu t c hi, vn vn.

Khng c cc yu cu v tiu chun c th (ngi Bulgari hay ngi Chu u) c


tm thy trong cc ti liu lin quan v vic cc nguyn t kim loi cha trong cc loi
tinh du. Tuy nhin, cc nguyn t nh Fe, Cr, Cu v Mn c th nh hng nhiu nht
n s n nh trong qu trnh lu tr do tnh xc tc ca chng, v hm lng Cd v Pb
d b hn ch do bi c tnh cao ca cc nguyn t ny. Ni chung, ty thuc vo vic
s dng cc loi du, cc tiu chun ca cc sn phm tng ng c quan st thc
phm, m phm, vn vn. Ch c mt vi bi vit lin quan n vic xc nh cc nguyn
t vi lng trong cc cc loi tinh du [14-16]. Mt trong s cc bi vit ny cn c vo
tro kh s b ca mu du sinh ra bi phng php ETAAS xc nh cc nguyn t vi
lng [14]. Cd, Cu, Pb, Zn, Mn c th c xc nh trong cc loi du cam qut bng
in th sau khi chit acid hydro-chloric v kt qu c so snh vi nhng nguyn t
ny thu c bng phng php ETAAS, sau khi ha m mu [15-16]. Phng php
ETAAS trc tip c s dng xc nh nh trong cc loi du hoa hng v hoa oi
hng v hm lng rt thp ca As c tm thy [17]. Ti liu kho st ca chng ti
ch ra rng khng c d liu c h thng v cc cp ca cc nguyn t vi lng trong
cc sn phm tinh du c sn xut t cc vng khc nhau Bungaria. V kha cnh
ny, khng c d liu no c cng b v kh nng ca cc phng php em li cho
vic xc nh cc nguyn t vi lng trong cc loi tinh du.
Mc nh ca cc nghin cu hin nay l thc hin phn tch cc sn phm tinh du
hoa oi hng v cm hoa oi hng t nhng cm hoa ny m t s di chuyn ca
cc nguyn t vi lng (Cd, Cr, Cu, Fe, Mn v Pb) trong cc cm hoa oi hng h
thng tinh du. Nh l bc u tin, cn thit xy dng mt tp hp cc phng php
cho ETAAS xc nh cc nguyn t vi lng trong du hoa oi hng. Bc th hai,
nhng cm hoa oi hng c ngun gc t ba khu vc kiu mu v cc loi du hoa oi
hng c sn xut t chng c phn tch. Hai khu vc cch xa khi nhng hot
ng cng nghip, l nhng vng tng i cha b nhim lng Zelenikovo ( phn
pha nam ngn ni Sredna Gona, mt a phng) v mt th trn Pavel Banya ( phn
pha bc ngn ni Sredna Gona, vi 4 a phng ring bit Atyovo, Kara, Rosena v
Chaliyata). Mt khu vc c t rt gn nh my luyn kim loi mu Plovdiv (khong
2km) (xem hnh 1). Mt mu du hoa oi hng c sn xut trong phng th nghim
(thit b Clavenger) cng c phn tch thit lp s tc ng ca quy trnh thit b
trn hm lng cc nguyn t vi lng trong sn phm cui. Nhng mu hoa oi hng
c ly t nh my chng ct ngay lp tc trc khi sn xut du v chng c acid
ha m khng qua bt c s x l s b no khc (khng ra trc v thi kh). Cc loi
du hoa oi hng c phn tch trc tip bng phng php ETAAS.
2. TH NGHIM
2.1. Thit b
S o lng quang ph hp th nguyn t ngn la c thc hin trn my quang
ph Perkin Elmer Zeeman 1100 B vi kh / ngn la acetylene. Thng s thit b c

nh gi khch quan t c t l tn hiu nhiu cao nht. S o lng quang ph


hp th nguyn t nhit in c thc hin trn my quang ph Perkin Elmer
Zeeman 3030 vi mt thit b phun m HGA-600. Cc ngun sng c s dng n
cathode rng cho Cr, Cu, Fe, Mn v Pb v mt n phng in in cc km cho Cd
(Perkin Elmer). Di quang ph l 0.7nm.
in phn nhng ng than ch graphite ph graphite vi Pt nh l s iu
chnh bn vng v nhng ng vonfram c ngm c s dng nh mt thit
b phun m. S iu chnh bn vng vi Pt t c bi 3 ln tim 40 l dung dch
iu chnh (NH4)2PtCl6, 1000 l/l trong 5% v/v HCl vi nhit ha tro 10000C v
nhit nguyn t ha 21000C. Ngm ng vonfram c thc hin nh sau: mt
ng graphite khng c bao ph bn tri trong dung dch Na2WO4 m/v trong
khong 24 ting sau khi kh nhit phng. ng c t nng theo chng
trnh nhit nh sau: 1. 1000C trong 30 giy, 2. 14000C trong 30 giy, 3. 26500C
trong 10 giy [18]. Cc dung dch mu (20 l) c a vo thit b phun graphite
dng mt tim mu t ng AS-60. Tn hiu hp th nguyn t thu c ghi li t
my in Anadex. Ch cc khu vc cao im c s dng nh lng.Tham s
thit b ti u cho s o lng bng phng php ETAAS c nghin cu v
th hin trong bng 1.
Bng 1
Chng trnh nhit ti u HGA-600 cho s o lng bng phng php ETAAS ca
cc mu du
Bc Nhit , 0C
bin i, giy Gi, giy Tc kh, ml min-1
1
50
10
20
300
2
150
10
20
300
a
b
c
3
900 , 1200 , 1300
20
60
300
a
b
c
4
1400 , 2200 , 2500
0
3
0
a
Cd v Pb.
b
Cu, Mn v Fe.
c
Cr.
2.2. Thuc th
Tt c cc thuc th dng phn tch. Cc dung dch chun gc ca Cd, Cr, Cu, Fe, Mn
v Pb 100 g ml-1 l Titrisol, Merck trong 2% v/v HNO3. Cc dung dch chun lm vic
c chun b hng ngy bng cch pha long thch hp vi dung mi hu c (p.a.
Merck). Acid nitric thm vo c tinh ch bi s chng ct.
Dung dch chun gc ca Pt 980 g ml-1 trong 5% v/v HCl (Aldrich) c tim (40 l)
vo l than ch thu c lp bao ph bn vng. Nc ct hai ln c s dng trong
tt c cc th nghim.
2.3. Chun b mu

2.3.1. V c ha nhng mu thc vt


Nhng mu thc vt thu c t cc thit b chng ct ngay lp tc trc s lng
thc vt cho vo trong thit b v c v c ha m khng ra trc v thi kh.
Mu thc vt, cn 0.5g, cho vo trong beaker (cc) 25ml, thm vo 10ml acid nitric m
c, beaker c y bng mt mt knh ng h v qua m. Sau , un mu
nhit (1200C) tron b ct, vn cn c y bng mt knh ng h, cho n khi th
tch ca dung dch cn li 1-2ml. Sau khi lm ngui, thm vo 2ml H202 v mu c un
tip thm 10 pht na. Cui cng, dung dch mu th c chuyn qua ng ong 25ml
v thm nc ct hai ln va 25ml.
2.3.2. Chun b nhng mu du hoa oi hng
Nhng mu du hoa oi hng thu c sau khi kt thc qu trnh chng ct. Mu c
pha long trc tip trong mt cc mu t ng t trn cn phn tch, bng cch pha ch
mt lng tinh du v dung mi hu c (1,4-dioxan) thu c dung dch pha lang t
l 1 + 1, 1 + 2 m/m. Mu hoa oi hng c chun b bng cch thm vo mt th tch
thch hp (10-30l) ca dung dch chun tinh khit. Cc cc c y kn bng Parafilm
v c lc c dung dch ng nht; cc mu c pha long phi c xc
nhn n nh t nht 1 tun nhit thng. Cc cc ch c m trc khi thc hin
cc php o trnh dung mi hu c bay hi khng kim sot.
Bng 2
Hm lng nguyn t, ng g-1 trong cm hoa oi hng v du hoa oi hng (3 phng
php xc nh song song)
Cc khu vc

Cc v tr

Hm lng nguyn t, gi tr trung bnh s (ng g-1)

Inflorescence: cm hoa
Oil: Du
Laboratory produced lavender oilb : du hoa oi hng c sn xut trong phng th
nghim.
b

Cm hoa t Zelenikovo.

kt qu trong g g-1

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