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Methodologies for Food Fraud

Others | 2019 | Agilent TechnologiesInstrumentation
GC/MSD, LC/MS
Industries
Food & Agriculture
Manufacturer
Agilent Technologies

Summary

Importance of the topic


Food fraud undermines consumer trust, poses health risks, and drives regulatory actions worldwide. High-profile incidents—from the 2007 melamine pet food scandal to widespread adulteration of extra virgin olive oil, rice, tea, spirits, and seafood—highlight the need for robust analytical strategies. Detecting economically motivated adulteration (EMA) protects public health, ensures product authenticity, and secures fair trade.

Objectives and study overview


This guide presents state-of-the-art methodologies for food fraud detection, covering spectroscopic, spectrometric, chromatographic, elemental, genomic, and chemometric approaches. It emphasizes multivariate statistics and sample class prediction models to discriminate authentic from adulterated samples, balancing cost, portability, and analytical performance.

Methodology and instrumentation


The paper reviews key techniques and instruments:
  • Spectroscopic methods: FTIR (mid- and near-infrared), handheld NIR, Raman and spatially offset Raman spectroscopy (SORS) for rapid, field-deployable screening.
  • Chromatography and mass spectrometry: GC/MS (Agilent 8890/5977B), LC/Q-TOF (Agilent 6546), GC/TOF, GC/Q-TOF, and LC/Q-TOF workflows for fingerprinting volatile, semivolatile, and nonvolatile markers.
  • Elemental analysis: ICP-MS (Agilent 7900), ICP-OES (Agilent 5110), and isotope-ratio MS for trace-element profiling and geographic origin determination.
  • Genomic testing: mtDNA barcoding (COI, rbcL, matK), PCR-RFLP, lab-on-a-chip capillary electrophoresis (Agilent 2100 Bioanalyzer), and next-generation sequencing for species authentication in seafood, meat, and plant products.
  • Feature finding and chemometrics: recursive feature extraction, alignment tools (AMDIS, XCMS, Profinder), multivariate analysis (PCA, PLS-DA, SVM, decision trees, neural networks), and sample class prediction with Agilent Mass Profiler Professional and Classifier.

Main results and discussion


Non-targeted workflows combined with targeted compound identification enhance detection of known and unknown adulterants. Key findings include:
  • Milk adulteration (water, whey, urea, melamine) characterized by distinct IR absorption bands and GC/MS markers, requiring data normalization and chemometrics to minimize false positives/negatives.
  • Olive oil authentication challenged by flavor defects and sophisticated fraud, addressed by HPLC and GC/MS screening of chlorophyll degradation products, diacylglycerol, pyropheophytin, and volatile markers.
  • Rice authenticity (Basmati, Jasmine) distinguished by volatile aroma compounds (2-acetyl-1-pyrroline, hexanal) and NIR/SORS screening with multiplicative scatter correction and spectral normalization.
  • Spirits and denatured alcohol detected in whiskey via handheld SORS at low ppm levels; portable FTIR and Raman expand field capabilities.
  • Tea origin determined by ICP-MS trace-element profiles and multivariate statistics (canonical variate analysis) separating regional and processing types.
  • Seafood species mixtures analyzed by DNA metabarcoding and lab-on-a-chip PCR-RFLP, enhancing identification in processed products.

Benefits and practical applications


The integration of portable and laboratory instruments with user-friendly chemometric software delivers:
  • Rapid, cost-effective field screening to triage samples before detailed lab analysis.
  • High-throughput, automated sample class prediction for routine quality control.
  • Robust detection of both known and unexpected adulterants through combined targeted and non-targeted approaches.
  • Improved geographic origin verification safeguarding protected designations of origin (PDO) and trade compliance.

Future trends and possibilities


Emerging directions include:
  • Miniaturization and further portability of high-resolution MS and IR instruments for on-site testing.
  • Advanced algorithms leveraging AI and cloud computing for real-time chemometric model updates and spectral library sharing.
  • Enhanced NGS workflows and molecular structure elucidation tools (e.g., Molecular Structure Correlator) for unknown compound identification.
  • Integration of lab-on-a-chip sample prep with handheld detectors for seamless point-of-care authenticity testing.

Conclusion


A multi-technique strategy combining spectroscopic screening, mass spectrometric fingerprinting, elemental profiling, genomic assays, and powerful multivariate statistics offers the most comprehensive defense against food fraud. Continued instrument innovation and user-focused software will further democratize advanced EMA methodologies, enabling laboratories and field teams to rapidly secure supply chains and protect consumers.

Reference


  • Barboza, D.; Barrionuevo, A. Filler in Animal Feed Is Open Secret in China. The New York Times 30 April 2007.
  • Litzau, J. J.; Mercer, G. E.; Mulligan, K. J. GC-MS Screen for the Presence of Melamine, Ammeline, Ammelide, and Cyanuric Acid. FDA Center for Veterinary Medicine, May 2007.
  • Bhalla, V.; et al. Melamine Nephrotoxicity: an Emerging Epidemic in an Era of Globalization. Kidney International 2009, 75, 774–779.
  • GC-MS Screen for the Presence of Melamine, Ammeline, Amelide, and Cyanuric Acid. U.S. FDA, LIB No. 4423, vol. 4, October 2008.
  • FDA Notice of Public Meeting on Economically Motivated Adulteration. 74 Fed. Reg. 15,497 (April 6, 2009).
  • Frankel, E. N.; et al. Imported “Extra Virgin” Olive Oil Often Fails Standards. UC Davis Olive Center, July 2010.
  • Cord, C. 80 Percent is the New 69 Percent. Olive Oil Times Nov. 30, 2016.
  • Ayton, J.; Mailer, R. J.; Graham, K. The Effect of Storage Conditions on Extra Virgin Olive Oil Quality. RIRDC April 2012, 12/024.
  • Morales, M. T.; Luna, G.; Aparicio, R. S. Comparative Study of Virgin Olive Oil Sensory Defects. Food Chem. 2005, 91(2), 293–301.
  • Stein, S. E.; Scott, D. R. Optimization and Testing of Mass Spectral Library Search Algorithms. J. Amer. Soc. Mass Spectrom. 1994, 5(9), 859–866.
  • Taro, Q.; et al. New Investigator Tools for Two-Dimensional Chromatography. Chromatography Today 2018, 13–18.
  • Smith, C. A.; et al. XCMS: Processing Mass Spectrometry Data for Metabolite Profiling. Anal. Chem. 2006, 78(3), 779–782.
  • Hjelmeland, A. K.; et al. Chemical and Sensory Profiles of Cabernet Sauvignon Wines. Am. J. Enol. Vitic. 2013, 64(2), 169–179.
  • Bradbury, L. M.T.; et al. The Gene for Fragrance in Rice. Plant Biotechnol. J. 2005, 3, 363–370.
  • Bergman, C. J.; et al. Rapid GC Technique for Quantifying 2-Acetyl-1-Pyrroline in Rice. Cereal Chem. 2000, 77(4), 454–458.
  • Grimm, C. C.; et al. Screening for 2-Acetyl-1-Pyrroline in Rice Headspace. J. Agric. Food Chem. 2001, 49, 245–249.
  • Yannell, K. E.; Cuthbertson, D. Food Authenticity Testing with Agilent LC/Q-TOF. Agilent Tech. App. Note 5994-0694EN, March 2019.
  • WTO TRIPS Agreement Articles 22, 23. WTO Analytical Index, 2018.
  • Ibanez, J. G.; et al. Metals in Alcoholic Beverages: Review of Sources, Removal, Analysis. J. Food Compos. Anal. 2008, 21, 672–683.
  • Förstel, H. The Natural Fingerprint of Stable Isotopes – Use of IRMS to Test Food Authenticity. Anal. Bioanal. Chem. 2007, 388, 541–544.
  • Drivelos, S. A.; Georgiou, C. A. MultiElement and MultiIsotope-Ratio-Analysis for Geographic Origin. Trends Anal. Chem. 2012, 40, 38–51.
  • Nelson, J.; Hopfer, H. Authentication of Specialty Teas: Application Note. Food Qual. Saf. 2019, Dec/Jan, 32–33.
  • Woods, G. Measurement of Trace Elements in Malt Spirit Beverages by ICP-MS. Agilent App. Note 5989-7214EN, August 2007.
  • Moore, J. C.; Spink, J.; Lipp, M. Database of Food Fraud and Economically Motivated Adulteration from 1980 to 2010. J. Food Sci. 2012, 77(4), R118–R126.
  • Santos, P. M.; Pereira-Filho, E. R.; Rodriguez-Saona, L. E. Hand-Held Infrared Spectrometers in Bovine Milk Analysis. J. Agric. Food Chem. 2013, 61, 1205–1211.
  • Pasquini, C. New Infrared Spectroscopy: Fundamentals and Applications. J. Braz. Chem. Soc. 2003, 14(2), 198–219.
  • Muthayya, S.; et al. Global Rice Production, Supply, Consumption. Ann. N.Y. Acad. Sci. 2014, 1324, 7–14.
  • Ellis, D. I.; et al. Handheld SORS Device for Counterfeit Alcohol Detection. Sci. Rep. 2017, 7, 12082.
  • Izake, E. L. Forensics and Homeland Security Applications of Portable Raman Spectroscopy. Forensic Sci. Int. 2010, 202(1-3), 1–8.
  • Dooley, J.; et al. Improved Fish Species Identification by Lab-on-a-Chip. Food Control 2005, 16, 601–607.
  • Hebert, P. D.; et al. Biological Identifications Through DNA Barcodes. Proc. Biol. Sci. 2003, 270(1512), 313–321.
  • Ratnasingham, S.; Hebert, P. D. BOLD: Barcode of Life Data System. Mol. Ecol. Notes 2007, 7, 355–364.
  • Handy, S. M.; et al. Evaluation of Agilent Bioanalyzer-Based DNA Fish Identification. Food Control 2017, 73, 627–633.
  • Cespedes, A.; et al. Flatfish Species Identification Using PCR-RFLP of Cytochrome b. J. Food Sci. 1998, 63, 206–209.
  • Wattoo, J. I.; et al. DNA Barcoding of rbcL and matK in Plants. Adv. Life Sci. 2016, 4(1), 3–7.
  • CBOL Plant Working Group. A DNA Barcode for Land Plants. PNAS 2009, 106(31), 12794–12797.
  • Garrett, S.; Clarke, M. Bioanalyzer for Basmati Rice Authenticity. Agilent App. Note 5989-6836EN, 2007.
  • Wong, E. H.; Hanner, R. H. DNA Barcoding Detects Market Substitution in Seafood. Food Res. Int. 2008, 41(8), 828–837.
  • Xing, R-R.; et al. Next Generation Sequencing for Species ID in Meat and Poultry. Food Control 2019, 101, 173–179.
  • Dymerski, T.; Chmiel, T.; Wardencki, W. Invited Review: An Odor-Sensing System for Foodstuff Studies. Rev. Sci. Instrum. 2011, 82, 111101–111132.
  • Śliwińska, M.; et al. Food Analysis Using Artificial Senses. J. Agric. Food Chem. 2014, 62, 1423–1448.
  • Pillonel, L.; et al. Determination of Geographic Origin of Emmental Cheese: GC/MS and e-Nose. Eur. Food Res. Technol. 2003, 216, 179–183.
  • Bertelli, D.; et al. Detection of Honey Adulteration by 1D and 2D HR-NMR. J. Agric. Food Chem. 2010, 58, 8495–8501.
  • Faul, F.; et al. G*Power 3.1: Power Analyses for Correlation and Regression. Behav. Res. Methods 2009, 41(4), 1149–1160.
  • Johnson, W. E.; Li, C. Adjusting Batch Effects in Microarray Data. Biostatistics 2007, 8(1), 118–127.
  • Schultz-Trieglaff, O.; et al. Statistical Quality Assessment and Outlier Detection for LC-MS. BioData Mining 2009, 2:4.
  • Dunn, W.; et al. Importance of Experimental Design and QC in Untargeted Metabolomics. Bioanalysis 2012, 4(18), 2249–2264.

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