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HMF in HONEY. Biagio Fallico, Elena Arena, Mario Zappal à , Antonella Verzera University of Catania - University of Messina (Italy) 3 rd AOAC Europe – EURACHEM Symposium 3 March 2005 Brussels. 3 rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005. HONEY REGULATIONS.
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HMF in HONEY Biagio Fallico, Elena Arena, Mario Zappalà, Antonella Verzera University of Catania - University of Messina (Italy) 3rd AOAC Europe – EURACHEM Symposium 3 March 2005 Brussels
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 HONEY REGULATIONS • Codex Alimentarius Commission • Joint FAO/WHO Food Standard Programme • (24th session, Geneva, 2-7 July 2001) • Report of the seventh session of the Codex Committee on Sugars • (ALINORM 01/25, London 9-11 Feb. 2000) • EC Directive 2001/110 Relating to Honey
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 ALINORM 01/25 • Essential Composition and Quality Factors • Chemical composition (moisture, sugars, insoluble solids, conductivity) • Contaminants • Hygiene • Labelling • Methods of sampling and analysis
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 ALINORM 01/25 • Additional Composition and Quality Factors • Free acidity • Diastase activity • Hydroxymethylfurfural (HMF) • After processing and/or blending: • 40 mg/Kg • 80 mg/Kg for honey from Countries or Regions with tropical ambient temperatures
6.a Diastase (Schade scale) • 8 (in general, except bakers honey) • 3 (honey with low natural enzyme content (e.g. citrus honey) and a HMF level not higher than 15 mg/kg. • 6.b HMF • 40 mg/Kg • 80 mg/Kg in honeys of declared origin from Regions with tropical climate 3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 • EC Directive 2001/110 • Annex II – Composition criteria for honey • sugars • moisture • water insoluble solids • electrical conductivity • free acids • Diastase activity and HMF (determined after processing)
HEATING TREATMENTS Citrus (Citrus Aurantum L.) Chestnut ( Castanea Sativa L.) Eucalyptus (Eucalyptus Camaldulensis L.) Sulla ( Hedysarium Coronarium L.) 3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 Analyses: moisture, glucose, fructose, pH, free acids, lactones, total acidity, conductivity, ash, diastase and HMF Heating at: 50 °C up to 144 h (6 days); 70 °C up to 96 h (4 days) 100°C up to 60 h (2.5 days)
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 Chemical composition of the Unifloral honeys
16000 12000 mg/kg 8000 4000 0 0 4 8 12 24 36 48 60 hours of heating Chestnut Eucaliptus Citrus Sulla 3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 HMF formation during heating at 100°C
Chestnut Eucaliptus Citrus Sulla 3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 HMF formation during heating at 70°C
30 25 20 mg/Kg 15 10 5 0 0 48 60 72 84 96 108 120 144 hours of heating Chestnut Eucaliptus Citrus Sulla 3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 HMF formation during heating at 50°C
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 • Influencing factors on HMF levels at 50°C • (Results applying ANOVA and Multiple linear regression model analyses) • Main factors: • pH of honey • temperature and time of heating • Specific factors: • Eucalyptus and Sulla were correlated to acidity • Citrus was correlated, at the same time, to: • time, pH and free acidity.
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 HMF is clearly an heating index, but the statement that the amount of HMF is independent of honey type and composition could be wrong. Among the studied honeys, Citrus, at the same time of heating, gives the highest amount of HMF
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 Citrus honey is a low natural enzyme content 9.3±2.7 (Range: 3.4-16.3) D.U. (Persano Oddo et al., 1995, 1999) The half life of Diastase in honey at 30°C is: 6/7 months This means 15 mg/kg as HMF limit
Storage of Citrus Honey (244°C) 75 60 45 HMF (mg/Kg) 30 15 0 Months 0 5 6 8 10 15 17 18 Citrus 1 Citrus 2 Citrus 3 3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 • This does not sound as “scientific based” because: • a very low limit when there is a natural attitude to • form HMF, independently from heating • at the same time, honeys of different origin (chestnut) • can be overheated without reaching the limit (40 mg/Kg).
High honeys sampling levels in 6 months 35 samples (25 citrus) EU Alert 10 not conform samples 3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 Practical consequences (2004):
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 Practical consequences (2004): Direct Effects 10 criminal proceedings 1000€ each as penalties Legal expenses Product declassification or destruction • Side Effects • costumers complaints • No honey to sell • Toxic or contaminated samples
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005 Conclusions: More attention to: Hygiene aspects and Contaminants Eliminate the limit of 15 mg/kg for low enzyme honeys Correlate HMF limits to chemical parameters of honeys and not to the diastase activity