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timization of polyphenols extraction from spruce bark
Esakkiammal Sudha Esakkimuthu 1, Kelly Peeters 1,3, Ana Miklavčič Višnjevec 2,
Črtomir Tavzes 1,3, David DeVallance 1,2 , Andreja Kutnar 1,3
1. InnoRenew CoE, Livade 6, 6310 Izola, Slovenia. sudha.esakkimuthu@innorenew.eu, kelly.peeters@innorenew.eu,
crtomir.tavzes@innorenew.eu, david.devallance@innorenew.eu, andreja.kutnar@innorenew.eu
2. University of Primorska, Faculty of Mathematics, Natural Sciences and Information Technologies, Glagoljaška 8, SI-6000 Koper,
Slovenia. ana.miklavcic@famnit.upr.si, david.devallance@famnit.upr.si
3. University of Primorska, Andrej Marušič Institute, Titov trg 4, 6000 koper, Slovenia kelly.peeters@iam.upr.si,
andreja.kutnar@iam.upr.si
Spruce is a widely used raw material in the pulp and paper industry and produces a considerable amount
of biomass waste. As with most woody biomass used for pulp and paper, the removed bark from Spruce
ends up being a low-value by-product. In spruce, the bark constitutes 10-15% total weight of tree stems
and is detrimental in the pulping process and has to be removed before processing. Once removed, the
bark is generally used as an energy source. Extraction of commercially viable compounds from the bark
before burning is an interesting value-added option. The bark is heterogenous both morphologically
and chemically and contains cellulose, hemicelluloses, pectins, lignin and various extractives in different
proportions.
Spruce bark is a renewable source of biologically active compounds. More than 60 antioxidant compounds
isolated from spruce bark including piceid, astringin, quercetin and resveratrol. These polyphenolic
compounds showed anti-inflammatory, anti-tumor, antioxidant, antiaging properties, and therefore, are
potential ingredients for cosmetics, food and pharmaceutical industries. The present study focused on
the extraction of polyphenols from dry bark using hot water extraction and magnetic bead adsorption
and separation methodology. The extraction efficiency of polyphenols from the bark was evaluated by
adjusting extraction time, particle size (>38µm,>106µm,>150µm, >425µm) and different concentrations of
magnetic beads (Fe3O4, Fe3O4 modified with citric acid). The leached polyphenols from the magnetic
beads were identified and quantified using HPLC-DAD-ESI-MS/MS. The results indicated that polyphenol
extraction improved with larger particle sizes and high temperatures (90°C). Additionally, the polyphenols
with the highest peaks were identified as amurensin, 5-hydroxyconiferaldehyde, poncirin, gentisic acid,
gallic acid, epigallocatechin, vanillic acid, dihydrorobinetin, rutin and erybradein B. The results of the
research indicated that there exists future potential in extracting viable polyphenol compounds from
Spruce bark using hot water extraction at high temperatures on larger bark particles.
Keywords: bark, polyphenols, extraction, HPLC-DAD-ESI-MS/MS
Acknowledgement
Authors acknowledge the European Commission for funding the InnoRenew project (grant agreement
#739574) under the H2020 Widespread-2-Teaming programme and the Republic of Slovenia (investment
funding from the Republic of Slovenia and the European Regional Development Fund) as well as ARRS
research project J4-1767 and Marie Skłodowska-Curie grant MSCA-IF-101031402.
INNORENEW COE INTERNATIONAL CONFERENCE 2021
42
Esakkiammal Sudha Esakkimuthu 1, Kelly Peeters 1,3, Ana Miklavčič Višnjevec 2,
Črtomir Tavzes 1,3, David DeVallance 1,2 , Andreja Kutnar 1,3
1. InnoRenew CoE, Livade 6, 6310 Izola, Slovenia. sudha.esakkimuthu@innorenew.eu, kelly.peeters@innorenew.eu,
crtomir.tavzes@innorenew.eu, david.devallance@innorenew.eu, andreja.kutnar@innorenew.eu
2. University of Primorska, Faculty of Mathematics, Natural Sciences and Information Technologies, Glagoljaška 8, SI-6000 Koper,
Slovenia. ana.miklavcic@famnit.upr.si, david.devallance@famnit.upr.si
3. University of Primorska, Andrej Marušič Institute, Titov trg 4, 6000 koper, Slovenia kelly.peeters@iam.upr.si,
andreja.kutnar@iam.upr.si
Spruce is a widely used raw material in the pulp and paper industry and produces a considerable amount
of biomass waste. As with most woody biomass used for pulp and paper, the removed bark from Spruce
ends up being a low-value by-product. In spruce, the bark constitutes 10-15% total weight of tree stems
and is detrimental in the pulping process and has to be removed before processing. Once removed, the
bark is generally used as an energy source. Extraction of commercially viable compounds from the bark
before burning is an interesting value-added option. The bark is heterogenous both morphologically
and chemically and contains cellulose, hemicelluloses, pectins, lignin and various extractives in different
proportions.
Spruce bark is a renewable source of biologically active compounds. More than 60 antioxidant compounds
isolated from spruce bark including piceid, astringin, quercetin and resveratrol. These polyphenolic
compounds showed anti-inflammatory, anti-tumor, antioxidant, antiaging properties, and therefore, are
potential ingredients for cosmetics, food and pharmaceutical industries. The present study focused on
the extraction of polyphenols from dry bark using hot water extraction and magnetic bead adsorption
and separation methodology. The extraction efficiency of polyphenols from the bark was evaluated by
adjusting extraction time, particle size (>38µm,>106µm,>150µm, >425µm) and different concentrations of
magnetic beads (Fe3O4, Fe3O4 modified with citric acid). The leached polyphenols from the magnetic
beads were identified and quantified using HPLC-DAD-ESI-MS/MS. The results indicated that polyphenol
extraction improved with larger particle sizes and high temperatures (90°C). Additionally, the polyphenols
with the highest peaks were identified as amurensin, 5-hydroxyconiferaldehyde, poncirin, gentisic acid,
gallic acid, epigallocatechin, vanillic acid, dihydrorobinetin, rutin and erybradein B. The results of the
research indicated that there exists future potential in extracting viable polyphenol compounds from
Spruce bark using hot water extraction at high temperatures on larger bark particles.
Keywords: bark, polyphenols, extraction, HPLC-DAD-ESI-MS/MS
Acknowledgement
Authors acknowledge the European Commission for funding the InnoRenew project (grant agreement
#739574) under the H2020 Widespread-2-Teaming programme and the Republic of Slovenia (investment
funding from the Republic of Slovenia and the European Regional Development Fund) as well as ARRS
research project J4-1767 and Marie Skłodowska-Curie grant MSCA-IF-101031402.
INNORENEW COE INTERNATIONAL CONFERENCE 2021
42
