1. Evaluation of the application of nanofiltration to concentrate the hydroethanolic extract obtained from grape juice marc
N. B. EITEL, A. P. G. CRUZ, L. F. M. DA SILVA, S. P. FREITAS, L. M. C. CABRAL
NATALIA BARBOSA EITEL

2. Outline Introduction Materials & Methods Results Final Remarks
Acknowledments
References

3. Introduction Brazilians Grape Production Destinations (2000-2011)
(Adapted from Mello (2005), Mello (2008), Mello (2012))
What should we do with the grape marc???

4. Introduction Alternative grape marc applications:
Biochemical process feed stock (Bustamante et al., 2008)
Enzyme Production
Yeast Production
Raw Material for the cosmetic industry (Brazinha et al., )
In Brazil, it’s still used as agricultural inputs:
Animal feed
Fertilizer

5. Introduction Bioactive Compounds = Thermolabile
High cost of treatment
Large recovery potential
Rich phenolic composition
Great antioxidant potential
Biodegradation resistance
↓pH
↑ Phytotoxic compounds
Solution!
Membrane Separation Process: Nanofiltration!

6. Introduction Energy savings; Selectivity;
Separation of thermolabile compounds;
Simplicity of operation.
The use of solvents can hinder a membrane separation processes
Nanofiltration
Habert et al. (2006)
Tsui & Cheryan (2004)

7. Main Aims
To recover the phenolic compounds present in the grape marc, particularly flavonoids from the seeds and peels
To concentrate them

8. Acidified with citric acid
Materials & Methods
Grape Marc:
2010/2011 harvest courtesy of Aurora winery (RS/Brazil)
Hydroethanolic Extraction:
Extraction in semi-pilot scale with:
EtOH = 30%
pH = 4,0
Solvent: Substrate Ratio = 9
Acidified with citric acid

9. Materials & Methods Hydration without stirring at T = 30 ° C
Extraction at 50 ° C for 120 minutes at 48RPM
Centrifugation
Choice of the best NF conditions through limiting flux definition
Nanofiltration of the hydroethanolic extract .

10. Materials & Methods
Limiting flux at different temperatures at a flow rate of 700 L h-1
Limiting flux reached at 20°C and 30°C with pressure of 16 bar and at 40°C with a transmembrane pressure of 12 bar

11. Materials & Methods => NANOFILTRATION:
Spiral wound polyamide membrane modules system with filter area of 2,5m2;
40°C;
ΔP = 12 bar;
Javerage= 14,9 kg∙h‑1∙m-2;
Fed Batch until
VCF= V(Retantate) V(Permeate) ≥10
Main aims:
Concentrate the extract in bioactive compounds - RETENTATE
Recover the extraction solution - PERMEATE

12. Materials & Methods Quantification of bioactive compounds:
Total Phenolics (TP) – Singleton & Rossi (1965) modified by Georgé et. al. (2005)
Total and Monomeric Anthocyanins (TA/MA) – Giusti & Wrolstad (2001)
Antioxidant Activity (AA) – Rufino et. al. (2007) and RE et. al. (1999)

13. Results

14. Results
J = 23,8 kg.h‑1.m-2 Javerage= 14,9 kg·h‑1·m-2

15. Analytical Results Obtained For The Different Process Streams
Analysis
AA (μmol∙g-1 extract)
TP (mg∙100g-1 extract)
TA (mg∙100g-1 extract)
MA (mg∙100g-1 extract)
Feed
4,32 ±
0,13
55,40 ±
2,77
13,71 ±
0,07
10,90 ±
0,06
Retentate
49,02± 6,72
593,17 ±
25,64
155,23 ± 3,48
119,42 ±
4,13
Permeate
N/D
VCF
10,14 R
100%
N/D- Not Detected
VCF= V(Retantate) V(Feed) and R= 1− c Permeate c Feed ×100%

16. Results
Feed
Retentate
Permeate

17. Final Remarks
NF = attractive alternative for the concentration of bioactive compounds recovered from the grape marc through a hydroethanolic extraction:
40°C;
ΔP = 12 bar;
J average= 14,9 kg∙h‑1∙m-2
Other tests should be performed in larger scale to confirm these results
Suggestion: to determine the influence of other process parameters on its concentration and its permeate flux.

18. Acknowledgments

19. References
C. Brazinha et al. (2010), Filtration+Separation, 47, pp
P. Bridle et al. (1997), Food Chemistry, 58, pp
M. A Bustamante et al. (2008), Waste Management, 28, 372–380.
S. Georgé et al. (2005), J. of Agricultural and Food Chemistry, 53,
M. M. Giusti et al. (2001), Characterization and measurement of anthocyanins by UV-visible spectroscopy, In: Current Protocols in Food Analytical Chemistry, New York: Wiley.
A. C. Habert et al. (2006), In: Processos de Separação por Membranas, Rio de Janeiro, E-papers.
L. R. Mello (2005). Produção e Comercialização de Uvas e Vinhos – Panorama Bento Gonçalves, RS: EMBRAPA Uva e Vinho.
L. R. Mello (2008). Vitivinicultura brasileira: panorama Bento Gonçalves, RS: EMBRAPA Uva e Vinho.
L. R. Mello (2012). Vitivinicultura brasileira: Panorama Bento Gonçalves, RS: EMBRAPA Uva e Vinho.
R. Re et al. (1999), Free Radic. Biol. Med., 26,
M. S. Rufino et al. (2007), Metodologia Científica: Determinação da atividade antioxidante total em frutas pela captura do radical ABTS+, Comunicado Técnico Embrapa Agroindústria Tropical, 128.
V. L. Singleton et al. (1965), Am. J. Enol. Vitic., 16,
E. M. Tsui et al. (2004), J. of Membrane Science, 237, 61–69

20. Natalia Barbosa Eitel natalia.eitel@poli.ufrj.br
Thank you!
Natalia Barbosa Eitel