Romanian Biotechnological Letters Vol. 19, No. 4, 2014
Copyright © 2014 University of Bucharest Printed in Romania. All rights reserved
ORIGINAL PAPER
Romanian Biotechnological Letters, Vol. 19, No. 4, 2014 9561
Determination of Acrylamide in Bread by Gas Chromatography
– Tandem Mass Spectrometry
Received for publication, May 22, 2014
Accepted, June 20, 2014
MIOARA NEGOIȚĂ*, MONICA CATANĂ, ENUȚA IORGA, LUMINIȚA CATANĂ,
ALINA ADASCALULUI, NASTASIA BELC
National Research&Development Institute for Food Bioresources – IBA Bucharest, Romania
*Address corespondence to: 6 Dinu Vintila Street, District 2, 021102, Bucharest, Romania,
Phone: +4021.210.91.28; +4021.211.36.39, E-mail: mioaranegoita@yahoo.com
Abstract
In this paper are presented results of the experiments to develop a GC/MS/MSmethod to determine
acrylamide in bread.
Method is based on sample extraction in water, at acidicpH, purification with Carrez solutions and
centrifugation. The obtained extract is derivatized with potassium bromide and the saturated bromine-
water solution. Dibromurated derivative, 2,3-dibromopropionamide (2,3-DBPA) is extracted with ethyl
acetate:hexane (4:1, v/v) and then concentrated, purified and eluted with acetone. The obtained extract is
concentrated and residue of 2,3-DBPA is re-dissolved with ethyl acetate and triethylamineand coverted in
monobromurated derivate, 2-bromopropenamide (2-BPA), stable compound at GC/MS/MS analysis.
Separation, detection, identification and cuantification of 2-BPA are achieved by GC/MS/MS, on
capillary column based on polyethylene-glycol, 30 m x 0.25 mm x 0.25 µm, by using internal standard
method.Triple quadrupole mass spectrometeris operated positive electron impactionization mode(EI
+
),
and selectedmode of acquisition"Selected Reaction Monitoring - SRM"andmonitored transitions from a
precursor ion to a product ion.In order to quantify there were used transitions m/z 151→ 70 (for 2-BPA)
and m/z 154→73 (for 2-BPA-
13
C3), respectively.
There were assessed and estimated some of the performance characteristics of the method: linearity,
workingrange, linearity range, accuracy, precision and sensitivity.
Keywords: acrylamide, GC/MS/MS, performance characteristics, derivatization, bread
1. Introduction
In April 2002, scientists from the National Food Administration in Sweden, together
with those of the University of the Stockholm have raised fears nationwide, finding that
people consume acrylamide through their diet, the consumption of common foods, such
bread, biscuits, chips, coffee, etc., at much higher levels than allowed dose in drinking
water.Swedish results were quickly confirmed by working groups consisted of experts from
the World Health Organization, Food and Agriculture Organization, United Nations
Organization, National Center for Food Safety and Technology, etc. They identified and listed
research priorities and potential risks of acrylamide in food on human health (1).
Acrylamide has been classified by the International Agency for Research on Cancer
(IARC) as ‘probably carcinogenic for humans’(2) and recognized by the European Union
(EU) Scientific Committee on Food (3) as a genotoxic carcinogen.
Acrylamide, AA (CH2=CHCONH2, CAS79-0601) is a chemical process contaminant,
that is formed when foods are subjected to processes by roasting, baking at temperatures
above 120
0
C, the result of chemical reactions between a series of specific amino acids (e.g.
asparagine) and compounds with carbonyl groups (e.g. glucose, fructose, maltose). This
reaction, known as the Maillard reaction, gives to foods, on the one hand, the corresponding