7° Encontro Nacional
de Cromatografia
Grupo de Cromatografia
Sociedade Portuguesa de Qufmica
Departamento de Qufmica e Bioqufmica
Faculdade de Ci
e
ncias da Univ
e
rsidade do Porto
Titulo
7Q
Encon
tr
o
Naciona
l
de
Cromatografia
Coordena~ao
Aqu
i
les
Araujo Barros
J
ose
An
t
6n
i
o Rodrigues
Paulo Joaquim A
l
meida
L
uis Ferreira Guido
M
ar
i
a
Ines Rocha
L
u
i
s
Moreira
Gon~alvesManuela Maria Mor
e
ira
l
nes Ma
r
ia
Valente
D
aniel Oliveira
Carvalho
J
ose
de
Sousa
Ca
m
ara
J
ose Manuel
F
.
Nogueira
lmpressao e acabamento
Graficos
Reunidos
Rua
Alvares
Cabral,
22-324050
-
040 Porto
Edi~ao
Soc
iedade
Portugues
a
de Qui
mica
Uala
J
;
111ciro
de 2
0
1
2
Ti•
·
agem
275 e
xemplar
es
ISBN978-989-97 66
7-0-9
Deposito legal
338101/117° E
n
con
t
r
o N
ac
i
o
n
a
l
d
e Cr
om
a
to
g
r
a
fia
i
n
d
i
ce
Comprehensive two-dimensional gas chromatography-mass spectrometry (GCxGC-TOFMS}
.111alysis of volatiles in Brazilian Capsicum spp. chili peppers
I I PLC-DAD-MS analysis of Tempranillo grape seeds from different geographical origin
Cafc~lol, kahweol and related esters profile in espresso coffee
On the study of historical Arraiolos tapestries- a chromatographic and spectrometric approach
C h.11.1tlcrization of phenolic and polysaccharidic extracts of Ganoderma lucidum by
c h1omatographic techniques
/\nlloxldants in Pinus Pinaster and mycorrhizal fungi during the early steps of symbiosis
< lirornatographic techniques to obtain the biomolecules profile of inedible wild mushrooms
with .1nlioxidant value
~l'."onal variability of essential oils of Lavandu/a luisieri
/\n overview of the nutrients and non-nutrients present in the wild mushroom species most
.1pp1 ('Ciatcd in the Northeast of Portugal
(,C MS <111alysis of Portuguese propolis
Cylilll~ mulliflorus: phenolic characterization by HPLC-DAD, ESI-MSn and NMR combined nlt'thods
Ml'lll/10 oquat.ica: source of flavanone glycosides
V.lllcl~llon of a NP-HPLC-FLD method for tocopherol analysis in fresh lettuce
C lhll•lclcdzation of volatile compounds of passion fruit species of semi-arid region in the
1\1 olllll,lll Norl hcast
Vol.1lllc composition of Portuguese Oak and Portuguese Chestnut wood chips: their relevance
lo1 <H'nOIOf:l~dl purposes
0111' cl11111'""0"dl and comprehensive two-dimensional gas chromatography analysis of chestnut
.ul!i o,1k wood chips with different toasting degrees
No·w Ill' 111'1 C UV mcthot.l for the quantification of napthodianthrones from Hypericum species ( h,u ,,< tt•rlt<illon of Opuntia ficus spp. fractions obtained using Sephadex LH-20.
I if'h'llllhhllion of bisphcnol A in mussels using dispersive liquid-liquid microextraction and gas
t llltlllloiiOHfoiphy 111.1~~ ~pcctromclry
Clpllmlt.lllon of m \llu dcrivilliJation dispersive liquid-liquid microextraction for simultaneous
•·xt1 o11 tlo11 ul bhphC'nol 1\ ,tncl b1-.plwnol B in tuna canned followed by gas chromatography
-lio•vc•lnpnlo'llt .\lltl vo~hd,lllon ol .1 •.lmplt• .111cl ~cn~itive t-IPLC/FLD method for N-methyl
1 •lllfoillloilo".tll",lif ldo",ill .l!illlioil ll·,•,llf"• i>.l'•f'<i 011 ci''•IH'I~ivr <'XIrilrlion by QuEChERS
1
21
1
22
123
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12S
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7° E
n
con
tr
o Nacio
n
a
l
de C
rom
a
t
ograf
i
a
i
n
d
i
ce
New strategy to enhance the extraction efficiency of polyphenols from dietary vegetables using
a modified QuEChERS combined with UHPLC-PDA system
A selective and fast method for the quantitative determination of chloroanisoles in wines using
solid phase microextraction and gas chromatography-quadrupole mass spectrometry
Development of a QuEChERS-based extraction method for Ochratoxin A analysis in bread by
LC-FLD
GC-FID and GC-MS as a tool to screen the influence of wood ageing technologies in the brandies odourless and odourant compounds
Honey sugars analysis by ion chromatography method with Integrated Pulsed Amperometric Detection (IPAD)
Ocurrence and bioacessibility of nitrates in baby foods
Avalia~ao dos nfveis de contamina~ao com patulina em diferentes fases do processamento
industrial da fruta
Desenvolvimento de um metodo de analise de melamina em produtos alimentares atraves de MISPE-HPLC-DAD
Quantification of wine ellagitanins by LC-ESI-MS/MS-multiple reaction monitoring Gas-diffusion microextraction: a deeper understanding of the process
Determination of free and total diacetyl in wine by HPLC-UV using gas-diffusion microextraction
Determination of pesticide residues in grapes and wine using Quechers and liquid
chromatography-diode-array detection
Recovery and analysis by HPLC-DAD of natural antioxidants from brewer's spent-grain
Analysis of acids and sugars in fruit-based drinks by SEC-l:JV-RI
Analysis of honey main sugars by size-exclusion chromatography Monitoring malolactic fermentation using HPLC-UV-RI
Determination of chloropropanols in water and food samples using ultrasound-assisted dispersive liquid-liquid microextraction with derivatization and GC-MS detection
Arsenic speciation in rice and fish using HPLC-ICP-MS
Solid-phase extraction followed by dispersive liquid-liquid microextraction for the sensitive
determination of ethylphenols species in wine
Fast detection of ~-lactam antibiotics in milk by isocratic HPLC elution
Chromatographic analysis of macro and micronutrients in the most widely appreciated
cultivated mushrooms
142
143
144
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P86. Analysis
of honey main
sugars by
size-exclusion
chromatography
Mara
E.
B.
C.
Sousa
0·
*, Ant6nio M. Pere
sa.b
, Lufs G. Dia
sa,
forge
Sa
Morai
s
0,Letfcia
Estev
inho
0,
Adelio
A.S.C.
Mach
a
doe
aCIMO- Escola Superior Agraria, lnstituto Politecnico de Bragan~a. Portugal, b LSRE -Laboratory of Separation and Reaction Engineering-Associate Laboratory LSRE/LCM, Escola Superior Agraria, lnstituto Politecnico de Bragan~a. Portugal, cLAQUIPAI-Departamento Quimica, Faculdade de Ciencias, Universidade
do Porto, Portugal •mcbdias@iol.pl
The
m
a
in
constituents of honey are
sugars,
mainly the monosaccharides
fru
ctose
and
glucose
(reducing
suga
rs),
which account
for
80% of the total mass, while the
disaccharide
s
(especially
s
ucrose
and maltose)
represent 10
%
. In
general, fructose
predominates (giving a sweeter taste
to honey
than sucrose), although,
in
some honeys,
glucose (that assigns a
less
sweet taste
than
sucrose
but more
than
maltose) may be
the
main
s
ugar. The
fructose/glucose
ma
ss
ratio is
a parameter that allows the identification
of
po
ss
ible
adulterations of
honey
,
by signaling abnormal
level
s
of
glucose
due to the
addition of commercial glucose or
syr
ups. lt
also allows assessing the crystallization
trend
of the honey,
a
lthough
the glucose/water ratio
p
rovides
a more accurate
indication
of this
behavior.
Therefore,
for
marketing
purposes,
the quantification
of glucose and
fructose
i
n
honey
is a key
factor for
establishing its quality.
Thi
s
work reports
the
validation of
a
method for determination of honey sugars by SEC to
be used
as control
in the
st
udy
of
their determination with an
e
lectronic
tongue.
A set of
honey
sa
mple
s
was
provided by
the
Portugue
se
National Federation
of
Be
ekee
per
s
to obtain a
national
sa
mplin
g
whi
c
h
s
howed
the
natur
a
l
composition
variability of Portuguese honeys.
The
analysis were carried out
with HPLC
e
quipment
from
Varian and a Supelcogel C-610H column,
se
lected
because the elution does not require
organic
so
lv
ents.
The target compounds to analyze were glucose and fructose for
whi
c
h
well
se
p
a
rat
ed
peaks were found in the chromatograms, which
included
ot
he
r
two, for a
mix
of polyssacharides and
unknown
substance(s).
The
results of a thorough validation
s
howed
that the
method
can
be
emp
loy
ed
for
quantifi
ca
tion
of these
two
s
u
ga
r
s in
honey
samp
le
s.
ANALYSIS
O
F HONEY MAIN
S
UGARS
BY S
IZE-EXCLUSION
C
HROMATOGRAPHY
Mara E
.
B
.
C
.
Sousa
&."
, A
n
t6nio M
.
Pere~·~'~,L
ais G
.
Dias9. Jo
rg
e SB Morais
&,
L
eticia
E
slevin
h
o
fl
r
A
d
f:lio
A.S.C.Machada
c
"CIMO • Esooaa ~dor Agnirfa. tnstltuto Politecn.co de Bragan98-, Portugal. • LSRE • Laboratory of Separallon and Reaction Engineering • As9oclale Laboratory LSREII..CM,
Escota Superior Aglliria, tns.tituto Pollte<:nlco de Bragan~. Portugal, ~LAOUIPAI • Oepartamento Ootmlca. faC\Ad&de de CiAnclas. llri'Versld&de do Potto. Portugal
Introduction
Main
constitu&nts of hon
ey
are sugar
s
:
' 80
%
fructose and gluc
os
e:
• 10% d~acchandes (especially sucrose and maltose).
Fructos& pr&dom
i
natGs
s
n
honey
I
n some.
g
l
ucose may be
t
OO main sugar
.
Fructos&/glucos&
mass
tabO:ldentJiicabOn
ofposs
l.
b
l
e
adultoratioos
of
honey,
• >1.3 will crystallize stowty or remam liquid.Objectives
HPLC method vahdabon for honey sugars determination
by SEC {slz&-exctusion Chromatography)
Referanoo method Jn the study of their detetmination with an atactronlc tongue.
Samples
!lar.eys l'lfl)•.'ld!ld by rMP • Pvtt;'}uesu c Cd111<tt :;(1 uf Bcu~:i
P.u~t.':J.li fr<1~1 dtllllfCfll P .t.~3 11:91tlb Sa!"'!p!llS lltC1)3f3!11Yl-DILUTION.
HPLC equipment
'Ja_"lan
Pro!ilar
22'
..
1Pump
Va."lar
Rl
-·
1
lrefrat:we
1ndcxOOtcctori
•metx:t!as@lol.pt
R
esul
t
s
1. COO"'pound id.entification- ret&ntlon timo-.
2.
Calibration- glucose and fructose. 3. Study of ACCURACY ao>d PRECISION:• 2 quality conttol solutloi\S;
• 3 honey sampl&s (different cotom). 4. T&n different honeys aJlalysed.
-
,
-
·
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1
-
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·
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·
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fnsacttla1h~..-
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Manual
;t!JI)CIOf ''l'llloop (11 LU IJlSoftwa.-o
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Supelcogel
C
610H
d•3Ccrr
x 7.amrr
0
1
GREEN CHEMICAL ANALYSIS
HPLC co
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d
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