biagio fallico, elena arena, mario zappalà, antonella verzeraaoaceurope.com/2005/fall.pdf ·...
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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 Symposium3 March 2005
Brussels
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
Additional Composition and Quality Factors
• Free acidity• Diastase activity• Hydroxymethylfurfural (HMF)
Essential Composition and Quality Factors
• Chemical composition (moisture, sugars, insoluble solids, conductivity)• Contaminants• Hygiene• Labelling• Methods of sampling and analysis
After processing and/or blending:
≤ 40 mg/Kg≤ 80 mg/Kg for honey from Countries or Regions with tropical
ambient temperatures
ALINORM 01/25
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005
EC Directive 2001/110
Annex II – Composition criteria for honey1. sugars2. moisture3. water insoluble solids4. electrical conductivity5. free acids6. Diastase activity and HMF (determined after processing)6.a Diastase
≥ 8 Schade scale≥3 in honeys with low natural enzyme content and HMF≤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
How much these limits in the present regulationsare “scientific sound”
OHOCH2 CHO
HMF
Fructose (or glucose)
endiol
-3 H2O
Statement: the amount of HMF in honey depends
only by time and temperature of heating and/or storage
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005
H+ Catalysed
HMF in unifloral honeys:
Effect of storage
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005
Effect of heating
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)
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
Chemical composition of the Unifloral honeys
1264131128193Electrical conductivity(µS)
1.23--5.95HMF (mg/kg)
10.833.927.37.6Diastase (DU)
25
22.5
3.4
Citrus
1832.511.4Total acidity (meq/kg)
15.5239.7Free acids (meq/kg)
3.43.75.9pH
SullaEucalyptusChestnutParameter
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005
Chestnut Eucaliptus Citrus Sulla
HMF formation during heating at 100°C
hours of heating
0
4000
8000
12000
16000
0 4 8 12 24 36 48 60
mg/
kg
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005
HMF formation during heating at 70°C
Chestnut Eucaliptus Citrus Sulla
0100200300400500600
0 4 8 12 24 48 60 72 84 96
hours of heating
mg/
kg
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005
HMF formation during heating at 50°C
Chestnut Eucaliptus Citrus Sulla
0
5
10
15
20
25
30
0 48 60 72 84 96 108 120 144
hours of heating
mg/
Kg
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005
Influencing factors on HMF levels at 50°C
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
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005
Storage of Citrus Honey (24±4°C)
0
15
30
45
60
75
0 5 6 8 10 15 17 18Citrus 1 Citrus 2 Citrus 3
HM
F (m
g/K
g)
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 toform HMF, independently from heating
• at the same time, honeys of different origin (chestnut)can be overheated without reaching the limit (40 mg/Kg).
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005
Practical consequences (2004):
Direct Effects10 criminal proceedings1000€ each penaltiesLegal expensesProduct declassificationor destruction
Side Effectscostumers complaints•No honey to sell•Toxic or contaminated samples
High honeys sampling levels
10 not conform samples
in 6 months35 samples (25 citrus)
EU Alert
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
3rd AOAC Europe, Eurachem Symposium, Brussels 3 March 2005