Outline General concepts Instruments Applications reflectance, - PowerPoint PPT Presentation

Outline  General concepts  Instruments  Applications  reflectance, absorption, fluorescence  Non-conventional instruments for absorption spectroscopy  Spectroscopy by mobile devices  Raman spectroscopy  The kitchen of the future 1

………… Steps towards multicomponent analysis Spectroscopy  Chemometrics  Classification maps  Library of ref. spectra / analytical data  Model for prediction of quality indicators  Validation  R 2

 Reflection spectroscopy  Meat  Cheese  Tomatoes  Honey  Surimi 3

Fiber optic spectroscopy for process control of beef Fiber optic reflectometer for online detection of beef premature browning FO probe M. O’Farrell et alii, IEEE Sensors J. , vol. 5, 2005, pp. 1407 M. O’Farrell et alii, IEEE Sensors J. , vol. 7, 2007, pp. 1685 4

Cheese – quality dry matter fat Č urda et alii, J. Food Eng. , vol. 61, 2004, pp.557-560 C.C. Fagan et alii, Int. Dairy J. , vol. 18, 2008, pp. 120-128 5

Surimi – quality protein content water content M.Uddin et alii, Food Chem. , vol. 96, 2006, pp. 491-495 6

Honey – adulteration pure - beet syrup adulterated - corn syrup 10-50% w/w G. Downey et alii, J. Near Infrared Spectr. vol. 11, 2003, pp. 447-456 T. Woodcock et alii, Food Chem., vol. 114, 2009, pp. 742-746 7

Tomato – nutraceutinc labelling of lycopene + lycopene

Tomato – nutraceutinc labelling of lycopene R 2 (cal) R 2 (val) RMSEC RMSECV mg/hg mg/hg 0,81 4,2 0,78 4,6 Calist a Volna 0,9 2,1 0,81 2,5

 Absorption spectroscopy  Milk  Tea  Olive oil  Wines  Tequila  Whisky 10

Milk – quality M. Kawasaki et alii, Comp. Electron. Agric. , vol. 63, 2008, pp.22-27 11

Tea – authentication & multianalytics from leaves from infusion  Multicomponent analysis of antioxidants and product features  Excellent correlation (R 2 >0.87) to polyphenols,caffeine,amino- acids, lignin Y. He et alii, J. Food Eng. vol. 79, 2007, pp. 1238-1242 S.He Yan, J. NIR Spectr. vol. 13, 2007, pp. 313-325 12

Extra virgin olive oil – adulteration sunflower olive sunflower-olive mixtures olive A.A. Christy et alii, Anal. Sci. vol. 20, 2004, pp. 935-940 G. Downey et alii, J. Agric. Food Chem. vol. 50, 2002, 5520-5525 13

Extra virgin olive oil – authentication Calabria Lombardy 0.2 Sicily DF 3 0 Tuscany -0.2 0.6 -0.5 0.4 0.2 0 0 0.5 -0.2 DF 2 DF 1 A.G. Mignani et alii, SPIE vol. 7003, 2008, pp. 700326-1/6 A.G. Mignani et alii, SPIE vol. 6585, 2007, pp. 65852C-1/6 14

Olive oil – correlation to nutritional factors Parameter Average content SECV R % Oleic Acid 74.4 % 2.5 % 0.91 % Palmitic Acid 11.9 % 1.7 % 0.87 % Palmitoleic Acid 0.8 % 0.4 % 0.81 % Palmitic + Stearic Acids 14.1 % 1.4 % 0.97 % Eptadecanoic Acid 0.1 % 0.05 % 0.70 % Eptadecenoic Acid 0.2 % 0.07 % 0.80 % Linoleic + Linolenic Acids 9.6 % 1.8 % 0.66 R = 0.87 R = 0.91 14 80 13 Estimated Palmitic Estimated Oleic 78 12 76 11 74 10 9 72 8 8 10 12 14 16 70 75 80 Oleic Palmitic A.G. Mignani et alii, SPIE vol. 7003 , 2008, pp. 700326-1/6 15

16 Our experiment with Chinese soy-bean oils

http://www.youtube.com/watch?v= aZEs9XK4PBU 17 Hogwash oil

Detection of hogwash oil in soy-bean oils using optical spectroscopy H: hogwash oil  S1: Arawana Dragonfish soy-bean oil  S2: soy-bean oil, local production  S3: Italian soy-bean oil  Mixs: 5%-10%-25%-50%-75% v/v  Replicas: 25%-50%-75% v/v and pure oils  18

Absorption spectroscopy – in transmission White LED Oil sample source in a vial Optical fiber spectrometer Transmitted spectrum

Detection of hogwash oil using full-band absorption spectroscopy Asterisks = validation points Asterisks = validation points 0.015 0 s3 s3h05 s3h10 h h 0.01 s3h25 s3h75 -5 s3h75 s3h75 s3h50 s3 s1h75 s2h75 s3 s1h75 s3h05 s2h75 s3h50 s3h50 s3h10 0.005 s3h25 PC 2 ( 4.3 % ) s3h25 Angle ( deg ) -10 s1h50 s1h50 s2h50 0 s1 s2h50 s2 -15 s2h75 s1h25 s3 -0.005 s1h25 s2h50 s2 s2h25 h s2h25 s2h10 s2h05 s2h25 s1 s1h10 -20 -0.01 s1h05 s1h75 s1 s2h10 s2 s1 s2h05 s2 s2 s3 s1h50 s1 s1h25 s1h05 -0.015 -25 s1h10 -0.1 -0.05 0 0.05 0.1 0 0.05 0.1 0.15 PC 1 ( 95.6 % ) Distance

Wines – process monitoring D. Cozzolino et alii, Biotech. Bioeng. , 2006, doi 10.1002/bit.21067 21

Wine – authentication 22

Tequila – fraud detection http://www.itequila.org O. Barbosa Garcìa et alii, Spectrochm. Acta A , vol. 66, 2007, pp. 129-134 PhotonicsIndia 2010 23

Whisky – authentication Area ID code Brand C Bruichladdich D Tobermory N Arran Islands T Ardbeg X Islay Mist Z Bunnahabhain A Macallan 10 G Stronachie H Ancnoc J Speyburn Highlands K Tomatin M Tomintoul R Deanston S Ben Riach W Balblair C1 Chivas Regal Commercial ‐ grade blends C2 Ballantines C3 Johnny Walker 24

Whisky – authentication 1.4 1.4 highlands highlands 1.2 1.2 islands islands comm. comm. 1 1 Absorbance Absorbance 0.8 0.8 0.6 0.6 0.4 0.4 0.2 0.2 0 0 250 300 350 400 450 500 550 600 1200 1300 1400 1500 1600 1700 1800 1900 Wavelength ( nm ) Wavelength ( nm ) 0.6 C C1 0.4 N Z C3 0.2 T D J S 0 C2 DF 2 R -0.2 K X M -0.4 W G A highlands -0.6 H islands blends -0.8 -1.5 -1 -0.5 0 0.5 1 DF 1 A.G. Mignani et alii, Sens.Act.B, 2012, vol. 171-172, pp. 458-462 25

Fluorescence spectroscopy - Milk AFB1 AFM1 PMT filter UV LED micro-cell filter 26

A portable fluorometer for the rapid detection of the carcinogenic M1 aflatoxin in milk – the instrumentation 120 120 120 Em.Filter 450nm Em.Filter 450nm UVLED+exc.filt 365nm UVLED+exc.filt 365nm 100 100 100 80 80 80 A.U. A.U. 60 60 60 40 40 40 20 20 20 0 0 0 300 300 300 350 350 350 400 400 400 450 450 450 500 500 500 550 550 550 600 600 600 650 650 650 700 700 700 750 750 750 Wavelength (nm) Wavelength (nm) AFM1 cell: quartz ultra-micro 6500 up to the legal limit 6000 Fluorescence signal alarm 5500 5000 (Counts) >50ppt 4500 4000 baby-food alert 3500 25-50ppt 3000 safe 2500 < 25ppt 2000 BLANK 125 ppt 25 ppt 50 ppt AFM1 Concentration 27

Milk – AFM1 monitoring by fluorescence meas. Adult food: AFM1 < 50 ppt 0.04 0.035 Corrected Normalized Output 0 50 0.03 100 250 0.025 0.02 0.015 0.01 0.005 10 0 400 450 500 550 600 650 5 Wavelength ( nm ) Miniaturized Miniaturized specrometer specrometer PC 2 ( 20.2 % ) 0 UV LED UV LED Optical fibers for Optical fibers for -5 illumination/detection illumination/detection -10 0  -cell for 90°-fluorescence  -cell for 90°-fluorescence 50 measurements measurements -15 100 250 -20 -15 -10 -5 0 5 10 15 C. Cucci et alii, Sens. Act. B, vol. 126, 2007, pp. 467-472 PC 1 ( 74.6 % ) A.G. Mignani et alii, SPIE vol. 7004, 2008, pp. 70045S-1/4 28