Detection of food fraud and

adulteration using novel

spectroscopic techniques

Xiaonan Lu
Assistant Professor
Food Science, UBC

Date: Nov. 7th, 2016

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Food fraud incidents

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Oceana Survey of US Seafood:

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 Food fraud incidents (con’t)

Figure 1. Food fraud incidents categorized by food group

(summarized by Food Protection and Defense Institute)

http://www.foodfraudresources.com/ema-incidents/ 4
 Definition of food fraud
• Food fraud
“the deliberate and intentional substitution,
addition, tampering, or misrepresentation of food,
food ingredients, or food packaging; or false or
misleading statements made for food products for
economic gain” – Spink and Moyer, 2011

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 Definition of food fraud (Con’t)
Motivation

Food Food
Quality Fraud1 Gain: Economic

Harm:
Food Food Public Health,
Safety Defense Economic, or
Terror
Unintentional Action Intentional
1Includes the subcategory of economically motivated
adulteration and food counterfeiting

Figure 2. Food protection risk matrix (Spink & Moyer, 2011)

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 Detriments of food fraud
 Economic loss of all parties (i.e. food industry,
government, consumers)
 Weaken consumers trust in food industry and
government
 Potential health risks
 allergens incorporated Food safety
 pathogen contaminated &
 poisoning Food defense

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 Traditional analytical techniques

LC/GC
• complex • complicated
• time • complicated instrumentation
consuming instrumentation • marker specific
• marker specific methodology
methodology
Sample
UV/DAD/MS
preparation

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 Traditional techniques (con’t)
• Fail to achieve:
 rapid analysis
 high-throughput screening
 user-friendly procedures
 detection of new types of deceptive behaviors

• Alternative:

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 Vibrational spectroscopies
• Raman and FT-IR spectroscopies
 Vibrational signals of functional groups
 Scattering or absorption spectra

symmetrical Asymmetrical Scissoring

stretching stretching

Figure 4. Representative
Rocking Wagging Twisting Raman spectra
Figure 3. Vibrational modes of molecules

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 Vibrational spectroscopies (con’t)
• NMR spectroscopy
 Vibrational signals of nucleus
 Resonance frequency spectra

Figure 5. Nucleic magnetic moment changes in Figure 6. Representative 1H

NMR spectroscopy NMR spectrum

NMR: nuclear magnetic resonance

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 Vibrational spectroscopies (con’t)
• Advantages
 Non/less-destructive
 Rapid
 Comprehensive chemical composition
 Unique fingerprinting features
 Able to emerge any extraneous materials

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Current projects in the lab

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• Detection and quantification of beef and pork offal in
ground beef meat

Three types of
pork offal
Raman spectrometer

Two types of
beef meat Chemometric analyses

FT-IR spectrometer
Three types of Figure 7. Schematic illustration of
beef offal experimental design 18
 Figure 8. Differentiation of beef meat and offal pure samples by
PCA models. Left, representative PCA for Raman spectroscopy;
right, representative PCA for FT-IR spectroscopy (n=30)

PCA: principal component analysis

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 • Detection and quantification of Sudan I in paprika
powder (Hu and Lu, 2016, Nature npj Science of Food, submitted)

Sudan I rotor
solution liquid extraction supernatant evaporation
centrifugation collection re-dissolve

solid & liquid Liquid-state

paprika mixture NMR tube
powder
HR MAS
solid-state
NMR rotor
Figure 10. Schematic illustration of experimental design

HR MAS: high resolution magic angle spinning

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 Liquid-state 1H NMR

1.2E+07

Spectra intensity at 8.57 ppm (AU)

1.0E+07 y = 19122x + 28542
R² = 0.9968

8.0E+06

6.0E+06

4.0E+06

2.0E+06

0.0E+00
0 200 400 600
Sudan I concentration in paprika powder (mg/kg)

Figure 11. Left, representative liquid-state 1H NMR spectra of Sudan I in paprika powder at
different concentrations (bottom to top: 20, 50, 100, 250 and 500 mg/kg); right, linear
regression of Sudan I concentration and NMR spectra intensity at 8.57 ppm (n=3)
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 HR MAS solid-state 1H NMR

7.0E+05

Spectra intensity at 7.89 ppm (AU)

6.0E+05 y = 268.73x - 13248
R² = 0.9885
5.0E+05

4.0E+05

3.0E+05

2.0E+05

1.0E+05

0.0E+00
0 500 1000 1500 2000 2500
Sudan I concentration in paprika powder (mg/kg)

Figure 12. Left, representative HR MAS solid-state 1H NMR spectra of Sudan I in paprika
powder at different concentrations (bottom to top: 225, 675, 1350, 1800 and 2250 mg/kg);
left, linear regression of Sudan I concentration and NMR spectra intensity at 7.89 ppm (n=3)
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 Next step…

Comparison and integration of

chemical library (UBC) &
molecular library (Guelph)

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 The DNA Barcoding Workflow – Library Building

Specimen Collection Data

Tissue Sample Photograph BOLD Systems

Web-Accessible Data and

Extract DNA PCR Amplify Sequence DNA Barcodes

Courtesy by Bob Hanner (University of Guelph) 24

 Acknowledgement
• Lu Food Safety Engineering Lab
• Yaxi Hu
• Prof. Eunice Li-Chan
• Dean Rickey Yada

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