Analytica Chimica Acta
Volume 520, Issues 1-2, 23 August 2004, Pages 207-215
First International Symposium on Recent Advances in Food Analysis, Prague, Czech Republic, Nov. 2003
Copyright © 2004 Elsevier B.V. All rights reserved. / Cited By in Scopus (39)
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Analysis of acrylamide in different foodstuffs using liquid chromatography–tandem mass spectrometry and gas chromatography–tandem mass spectrometry
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K. Hoenicke, , R. Gatermann, W. Harder and L. Hartig
Eurofins/Wiertz-Eggert-Jörissen GmbH, Stenzelring 14 b, D-2107, Hamburg, Germany
Received 16 December 2003;
Revised 12 March 2004;
accepted 12 March 2004.
Available online 21 May 2004.
Abstract
Acrylamide levels over a wide range of different food products were analysed using both liquid chromatography–tandem mass spectrometry (HPLC–MS–MS) and gas chromatography–tandem mass spectrometry (GC–MS–MS). Two different sample preparation methods for HPLC–MS–MS analysis were developed and optimised with respect to a high sample throughput on the one hand, and a robust and reliable analysis of difficult matrices on the other hand. The first method is applicable to various foods like potato chips, French fries, cereals, bread, and roasted coffee, allowing the analysis of up to 60 samples per technician and day. The second preparation method is not as simple and fast but enables analysis of difficult matrices like cacao, soluble coffee, molasses, or malt. In addition, this method produces extracts which are also well suited for GC–MS–MS analysis. GC–MS–MS has proven to be a sensitive and selective method offering two transitions for acrylamide even at low levels up to 1μgkg−1. For the respective methods the repeatability (n=10), given as coefficient of variation, ranged from 3% (acrylamide content of 550μgkg−1) to 12% (acrylamide content of 8μgkg−1) depending on the food matrix. The repeatability (n=3) for different food samples spiked with acrylamide (5–1500μgkg−1) ranged from 1 to 20% depending on the spiking level and the food matrix. The limit of quantification (referred to a signal-to-noise ratio of 9:1) was 30μgkg−1 for HPLC–MS–MS and 5μgkg−1 for GC–MS–MS. It could be demonstrated that measurement uncertainties were not only a result of analytical variability but also of inhomogeneity and stability of the acrylamide in food.
Author Keywords: Acrylamide; HPLC–MS–MS; GC–MS–MS; Sample preparation; Complex matrices; Inhomogeneity; Stability
Article Outline
1. Introduction
2. Experimental
2.1. Chemicals
2.2. Sample preparation
2.2.1. Routine extraction method
2.2.2. Alternative extraction method
2.3. HPLC–MS–MS analysis
2.4. GC–MS–MS analysis
2.5. Recovery tests and blank values
3. Results and discussion
3.1. Routine analyses of acrylamide
3.1.1. Extraction of acrylamide
3.1.2. Clean-up
3.2. Acrylamide analysis in complex matrices
3.3. Acrylamide analysis at low levels
3.4. Detection limit, recovery, and linearity
3.5. Causes for variability of acrylamide levels
3.5.1. Inhomogeneity of samples
3.5.2. Stability of acrylamide in food
4. Conclusion
Acknowledgements
References
Fig. 1. Acrylamide levels of a raw sugar sample analysed after routine extraction and PLE (ASE) at different temperatures.
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Fig. 2. MRM chromatograms of a potato chips sample obtained after routine extraction and HPLC–MS–MS analysis (concentration of acrylamide in the sample was 1049μgkg−1).
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Fig. 3. HPLC–MS–MS analysis of acrylamide in beet and cane molasses. MRM chromatograms of the transitions at m/z 72>55 (acrylamide) and 75>58 (d3-acrylamide) obtained (A) after routine extraction of beet and cane molasses and (B) after alternative extraction of beet molasses.
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Fig. 4. HPLC–MS–MS analysis of acrylamide in soluble coffee (concentration of acrylamide was 630μgkg−1). MRM chromatograms of the transitions at m/z 72>55 (acrylamide) and 75>58 (d3-acrylamide) obtained after (A) routine extraction and (B) alternative extraction.
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Fig. 5. MRM chromatograms of a baby food sample (acrylamide content of 10μgkg−1) obtained after alternative extraction using (A) HPLC–MS–MS analysis (monitored transitions at m/z 72>55 for acrylamide and 75>58 for d3-acrylamide) and (B) GC–MS–MS analysis (monitored transitions at m/z 89>55 and 89>72 for acrylamide and 92>75 for d3-acrylamide).
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Fig. 6. (A) Number of analysed samples and distribution of the methods used for analysis. (B) Mean values of acrylamide concentrations analysed in the respective food categories.
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Fig. 7. Analysis of a homogenised sample of potato chips () and a part of the same blend which contains predominantly dark particles (▪).
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Fig. 8. Decrease of acrylamide concentrations in a homogenised sample of potato chips over 100 days (n=28).
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Fig. 9. Decrease of acrylamide concentrations in a sulphurised 60° Brix sugar solution spiked with 1000μgkg−1 acrylamide () and control sample without addition of sulphite (▪).
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Table 1. Recovery (%) and coefficient of variation (CV) (%) of acrylamide for the different methods analysed in various food matrices at different spiking levels (n=3)
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Table 2. Mean, coefficient of variation (CV), and limit of quantification (LOQ) of acrylamide (n=10) for different food matrices determined using the respective extraction method and HPLC–MS–MS or GC–MS–MS analysis
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