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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

(3)

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~alves

Manuela 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,

22-32

4050

-

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

ISBN

978-989-97 66

7-0-9

Deposito legal

338101/11

(4)

7° 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

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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

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lo1 <H'nOIOf:l~dl purposes

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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.

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t llltlllloiiOHfoiphy 111.1~~ ~pcctromclry

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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

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12S

126

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131

l

132

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l

de C

rom

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ograf

i

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New strategy to enhance the extraction efficiency of polyphenols from dietary vegetables using

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A selective and fast method for the quantitative determination of chloroanisoles in wines using

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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)

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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

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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

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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

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1S6

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(5)

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.

(6)

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 g

luc

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

of

poss

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'

..

1

Pump

Va."lar

Rl

1

lrefrat:we

1ndcx

OOtcctori

•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.

-

,

-

·

~

-

1

-

' •

·

-

·

---

·---:.,Q,

Ii!)o

sa

ot

ha

n

des

? Orill-ll"iiiiii.(Q"CJCC11t'l«< cm...tr~o»tTJ.II(mti.Y'tf1)M Ot·~tcl#;lll,) Qt.q.mtlmtt~lru

---Ol

sa

c

c

h:afl

da

s -

fnsacttla1h~

..-

1

RhCO:ly'le nz: .•

Manual

;t!JI)CIOf ''l'llloop (11 LU IJl

Softwa.-o

Sic\' ciY•)matograp~y I'IC'b .. .:al1!:4. ,•crMon

6.4

Jvtes..

lt:.a

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thrt.tr..atograph)• culuz"ln o,•cl'l

(lu:My tontml SOiuliom fo!e:!~W't Gwmrti .stnUit . . . M ltllrt ... ~~bl~

-""·"

...

....

COLUMN

Supelcogel

C

610H

d•3Ccrr

x 7.amrr

0

1

GREEN CHEMICAL ANALYSIS

HPLC co

n

d

i

tions

C~h.tr!l !CMPQ•rlluu::.

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I~

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The

CNilrall ca

li

brallons are

acceplable

~

Re$u

lt

s

or

accuracy

and

precls

!

oo

are

at

ceplab

le

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T

OO

meltlod

can

be Mlployed

quaol

lflcallon

of

these

two

sug

n

io hOOOf

samplE!$.

F

ructosa

1n

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great

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ruclosetglucose mass

r

a

11o

in

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highflr

than

1.

3

4

.

Referências

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