FRIN-05058; No of Pages 7

Food Research International xxx (2014) xxx–xxx

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Food Research International

journal homepage: www.elsevier.com/locate/foodres

Hazelnut skin powder: A new brown colored functional ingredient

Kübra S. Özdemir a, Cemile Yılmaz a, Gökhan Durmaz b, Vural Gökmen a,⁎
a
Department of Food Engineering, Hacettepe University, 06800 Beytepe, Ankara, Turkey
b
Department of Food Engineering, İnönü University, Malatya, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: Hazelnut skin arises as a by-product in the roasting process of hazelnuts. This study aimed to investigate the
Received 18 October 2013 potential of its utilization as a brown colored functional ingredient. Chemical composition analyses revealed
Received in revised form 19 January 2014 that hazelnut skin is a very rich source of dietary fibers (67.7%) and phenolic compounds (233 mg GAE/g). Its
Accepted 24 January 2014
oil fraction (14.5%) was found to contain very high amounts of tocopherols (2.77 μg/g) and oleic acid (75.2%).
Available online xxxx
After defatting, coarse and fine hazelnut skin powders were obtained by low and high shear homogenization.
Keywords:
High shear homogenization was performed at different pressures (10, 20 and 30 ksi) for different pass cycles
Hazelnut skin (1, 3, 5 and 10). The powder samples were analyzed for particle size distribution, color, individual phenolic
Brown powder compounds, total phenolic content, and total antioxidant capacity. A desirable low micron particle size for the ha-
Dietary fiber zelnut skin for incorporation into food formulations was achieved by means of high shear homogenization,
Phenolic compounds meanwhile there was no significant change in phenolic composition and antioxidant capacity.
High-shear homogenization © 2014 Elsevier Ltd. All rights reserved.

1. Introduction Hazelnut skin offers potential for utilization as a coloring agent in

Hazelnut (Corylus avellana L.) belongs to Betulaceae family (Shahidi,
Alasalvar, & Liyana-Pathirana, 2007) and its edible nut is utilized in sev-
eral different ways including pastry, chocolate spread, ice cream, cereal
bar, cookie, nougat and cooking oil production (Platteau, De Loose, De
Meulenaer, & Taverniers, 2011). The world hazelnut production was
around 0.9 million tons/year in 2012. Turkey is the leading producer ac-
counting for about 70% of total supply (TMO, 2012). Hazelnut is a rich
source of polyphenolic components such as, flavan-3-ols, benzoic acids,
flavonols. (Jakopic et al., 2011; Solar & Stampar, 2011; Yurttas, Schafer,
& Warthesen, 2000). During processing of hazelnut, hazelnut skin and
other by-products including hard shell, green leafy cover and tree leaf
arise as waste materials (Del Rio, Calani, Dall'Asta, & Brighenti, 2011). Ha-
zelnut skin is removed from kernel after roasting process of hazelnut and
represents about 2.5% of total hazelnut kernel weight (Alasalvar et al.,
2009). It is an extremely rich source of fiber and several different poly-
phenolic compounds such as flavan-3-ols, phenolic acids and
procyanidins (Alasalvar et al., 2009; Locatelli et al., 2010; Montella,
Coisson, Travaglia, Locatelli, Malfa, Martelli, et al., 2013; Shahidi et al.,
2007). Hazelnut skin contains approximately 65% dietary fiber, 8% pro-
tein and 9% oil (Anil, 2007). Moreover, hazelnut skin is concentrated in
phenolic compounds, which makes it a significant waste product of the
hazelnut industry. The oil of the hazelnut skin could be extracted before
utilization of this cheap waste material in any other application.
Natural colorants have become popular day by day, because synthet-
ic colorants are perceived as undesirable or harmful (Tan et al., 2011).
foods with its natural brown color. However, its use for this purpose
needs further modification because of relatively larger flakes of ground
hazelnut skin. Particle size reduction could help to provide more
homogeneous color distribution when hazelnut skin was used in food
products. High shear homogenization treatment is an efficient and
alternative technology for particle size reduction and homogeneity.
The application of high shear homogenization treatment for decreasing
particle size has been previously reported in literature (Jong, 2013;
Kluge, Muhrer, & Mazzotti, 2012; Liu, Wu, Chen, & Chang, 2009). Also
chitosan nanofibers and cellulose nanofibrils from microcrystalline
cellulose and from wheat straw pulp were prepared by using high
shear homogenization (Lee, Chun, Kang, & Park, 2009; Liu, Chang,
Chen, & Wu, 2011; Zimmermann, Bordeanu, & Strub, 2010).
As an alternative brown coloring food ingredient, the compositional
and physical properties of hazelnut skin needs to be defined. Thus, this
study aimed to investigate (i) basic compositional properties of hazelnut
skin and its oil, and (ii) to produce brown-colored low-micron sized ha-
zelnut skin powder with high dietary fiber content and antioxidant that
could be used as a functional food ingredient. The effect of various pres-
sure and pass treatments of high shear homogenization on chemical and
physical properties of hazelnut skin fiber were also investigated.
2. Materials and methods
2.1. Chemicals and consumables

⁎ Corresponding author. Tel.: +90 312 2977108; fax: +90 312 2992123. Acetonitrile (HPLC grade), ethanol (HPLC grade), methanol, n-
E-mail address: vgokmen@hacettepe.edu.tr (V. Gökmen). hexane, gallic acid, Folin–Ciocalteu, potassium persulfate, ABTS reagent

0963-9969/$ – see front matter © 2014 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.foodres.2014.01.060

Please cite this article as: Özdemir, K.S., et al., Hazelnut skin powder: A new brown colored functional ingredient, Food Research International
(2014), http://dx.doi.org/10.1016/j.foodres.2014.01.060
2 K.S. Özdemir et al. / Food Research International xxx (2014) xxx–xxx
[2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid)], chlorogenic
acid, p-coumaric acid, ferulic acid, (+)-catechin, (−)epicatechin,
(−)-epicatechingallate,(−)-epigallocatechin gallate, (−)-gallocatechin,
and (−)-epigallocatechin, fatty acid methyl esters, 2-propanol, α-,β-,γ-
and δ-tocopherols were obtained from Sigma-Aldrich (Steinheim,
Germany). Formic acid (98%), hydrochloric acid, sodium hydroxide,
boric acid, sulfuric acid, diethyl ether and sodium carbonate were pur-
chased from Merck Co. (Darmstadt, Germany). Trolox [6-hydroxy-
2,5,7,8-tetramethylchroman-2-carboxylic acid] and citric acid mono-
hydrate were purchased from Fluka Chemie AG (Buchs, Switzerland).
Ethyl acetate and disodium hydrogen phosphate were purchased from
LAB-SCAN (Dublin, Ireland) and Acros (Geel, Belgium), respectively.
Amyloglucosidase and protease were obtained from Novozymes
(Bagsvaerd, Denmark).
Ultra-pure water was used throughout the experiments (Milli
Q-System, Millipore, Milford, MA, USA). Syringe filters (nylon,
0.45 μm) were supplied from Waters (Millford, MA). A fused silica
DB23 capillary column (60 m × 0.25 mm i.d. 0.25 μm film thickness)
was supplied from J&W Scientific (Folsom, CA). HICHROM 5C 18
(250 × 4.6 mm, Hichrom, Reading, UK) column and a NH 2 column
(5 μm 4.60 × 250 mm, LiChrospher) were used for analysis of indi-
vidual phenolic compounds and tocopherols, respectively.
2.2. Preparation of coarse and fine hazelnut skin powders
Raw hazelnuts (Tombul variety) were obtained from a local produc-
er in Turkey. After roasting at 150 °C for 30 min, brown skin of hazelnuts
was separated and ground with a domestic type grinder. Ground hazel-
nut skin was chemically characterized for its basic composition. Hazel-
nut skin was then extracted with hexane to obtain hazelnut skin oil
and defatted coarse hazelnut skin powder. A total of 10 g hazelnut
skin was extracted with 200 ml of hexane for 6 h. To obtain hazelnut
skin oil, hexane was removed by evaporation under a gentle stream
Fig. 1. Scheme for the treatments of hazelnuts to obtain coarse and fine hazelnut skin powder.
Please cite this article as: Özdemir, K.S., et al., Hazelnut skin powder: A new brown colored functional ingredient, Food Research International
(2014), http://dx.doi.org/10.1016/j.foodres.2014.01.060
on nitrogen. The skin oil was stored at −15 °C prior to its analyses for
fatty acid composition and tocopherols.
The coarse defatted powder was further treated by high shear ho-
mogenization to obtain fine powder of hazelnut skin. The coarse pow-
der was passed through a sieve having a mesh size of 40 (425 μm)
and suspended in water (1%). The suspension was pre-homogenized
using a low shear mixer (Heidolph, Silent M Crusher) at 25,000 rpm
for 8 min. Then, it was passed through a high shear microfluidizier
(M110P, Microfluidics, Newton, MA, USA) applying different pressures
(10, 20, 30 ksi) and pass cycles (1, 3, 5 and 10). After high shear homog-
enization, suspensions were lyophilized to obtain fine hazelnut skin
powders. The powder samples were stored at + 4 °C prior to their
chemical and physical characterizations. The scheme for the treatments
of hazelnuts to obtain defatted coarse and fine hazelnut skin powders is
shown in Fig. 1.
2.3. Analysis of hazelnut skin and hazelnut skin oil
2.3.1. Basic composition of hazelnut skin
Moisture (Method No: 925.10), ash (Method No: 930.05) and
protein (Method No: 984.13) contents were determined according to
Association of Official Analytical Chemists methods (AOAC, 1990).
Total protein content was calculated by multiplying the total nitrogen
content by a factor of 6.25. Dietary fiber (Method 32-07.01) analysis
was performed using American Association of Cereal Chemists methods
(AACC, 1991). To determine lipid content, ground hazelnut skins
(200 mg) were extracted with hexane (3 × 1 ml) and combined hexane
phases were evaporated under a gentle stream of nitrogen at 40 °C.
2.3.2. Fatty acid composition of hazelnut skin oil
Forty mg of oil was methylated with 3 ml of 60 g/L HCl in methanol
at 75 °C for 2 h. Fatty acid methyl esters (FAMEs) were extracted with
2 ml of hexane and dried over sodium sulfate. One μl of the FAMEs
was analyzed with an Agilent 7890 series gas chromatograph (Agilent
 K.S. Özdemir et al. / Food Research International xxx (2014) xxx–xxx
Company) equipped with a flame ionization detector and 7683B auto-
matic injector. A fused silica DB23 capillary column (60 m × 0.25 mm
i.d. 0.25 μm film thickness; J&W Scientific. Folsom. CA) was used. The
oven temperature was programmed as follows: 140 °C for 5 min in-
creased to 240 °C at 3 °C/min and kept at 240 °C for 10 min. The injec-
tion and detector temperatures were each 250 °C, the carrier gas was
helium, the flow rate was 30 ml/min, and the split ratio was 1/30.
FAME identification was based on retention times as compared with
those of the standard FAME mixture. Analysis was performed in tripli-
cate for each sample and the mean results were expressed as percentage
of peak area.
2.3.3. Tocopherols in hazelnut skin oil
Analysis was performed by using the same HPLC system used in phe-
nol analysis. Normal phase chromatographic separation was achieved
with a NH2 column (5 μm 4.60 × 250 mm. LiChrospher), and the column
temperature maintained at 30 °C. Oil samples were diluted ten times in
mobile phase (4% 2-propanol in hexane) and 20 μl injected to the
system. Elution was programmed as isocratic flow of 4% 2-propanol in
hexane for 20 min. Flow rate was set as 0.7 ml min−1 and the eluate
was monitored at 290 nm. α, β, γ, and δ-tocopherols were quantified
based on peak areas compared with external standards.
2.4. Physical and chemical characterizations of the coarse and fine hazelnut
skin powders
2.4.1. Color measurement
The color measurements were performed in CIE L*a*b* space using a
Minolta model CM-3600d color spectrophotometer (Osaka, Japan).
White and black calibration plates were used to calibrate the equipment
prior to color measurements. All measurements were taken under the
conditions of standard illuminant D65 and 10° observer. Color differ-
ence (ΔE) was estimated from the coordinates of the color by applying
the following equation:
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
ΔE ¼ ðΔL Þ2 þ ðΔa Þ þ ðΔb Þ2 :
2.4.2. Scanning electron microscope (SEM)
Samples placed on a stub were coated with a thin layer (10 nm) of
Au/Pd. A FEI Quanta 200F model SEM (Oregon, USA) instrument
equipped with a Schottky field emission gun for optimal spatial resolu-
tion was used to image the samples.
2.4.3. Particle size distribution
Particle size distribution of the samples was determined by wet dis-
persion module (Hydro 2000S) of a particle size analyzer (Malvern,
Mastersizer 2000SR). The Hydro 2000S module is equipped with a stir-
rer and an ultrasonic probe. In each measurement, the speed of stirrer
was fixed to 2000 rpm and 15 s and ultrasound treatment was applied
by means of an inbuilt probe. Particle size distributions were summa-
rized by the characteristic volume-based D(0.5) value which represents
% 50 of the total particle population.
2.4.4. Analysis of individual phenolic compounds
The soluble free, soluble conjugated and insoluble bound phenolic
compounds in samples were determined according to the procedure
described by Moore, Hao, Zhou, Luther, Costa and Yu (2005) with
some modifications. Sample (50 mg) was extracted with ethanol–
water (50:50, v/v) in three steps (1, 0.5, 0.5 ml) by mixing (5 min).
After centrifugation at 6080 ×g for 5 min, collected supernatant was fil-
tered through a 0.45 μm nylon filter into a vial to determine soluble free
phenolic compounds. The insoluble phenolic compounds in the residue
and conjugated phenolic compounds in collected extracts were released
by alkaline hydrolysis using 4N NaOH for 4 h at room temperature. After
Please cite this article as: Özdemir, K.S., et al., Hazelnut skin powder: A new brown colored functional ingredient, Food Research International
(2014), http://dx.doi.org/10.1016/j.foodres.2014.01.060
3
the pH was adjusted to 2.0 by 6N HCl, the hydrolysates were extracted
with ethyl acetate and diethyl ether (1:1, v/v) four times. The combined
extracts were evaporated under N2 stream at 30 °C to dryness. The final
residues were re-dissolved in 1 ml of ethanol–water (50:50, v/v) mix-
ture. After they were filtered through a 0.45 μm nylon filter, they trans-
ferred into vials prior to HPLC–MS analysis.
Chromatographic analysis was performed on an Agilent 1200 HPLC
system consisting of a photodiode array detector, quaternary pump,
autosampler, a temperature controlled column oven and equipped
with an Agilent 6130 MS detector. Separation was performed on a
HICHROM 5 C18 column using a gradient mixture of solvent A (1.0%
formic acid in water) and solvent B (1.0% formic acid in acetonitrile)
at a flow rate of 0.7 ml/min at 30 °C with the following gradient profile:
0–8 min; linear gradient elution from 10 to 30% B, 8–10 min; isocratic
elution of 30% B, 10–12 min; linear gradient elution from 30 to 10% B,
and 12–20 min; isocratic elution of 10% B. The injection volume was
10 μl. The electrospray source had the following settings: drying gas
(N2) flow of 13 l/min at 325 °C, nebulizer pressure of 40 psig, capillary
voltage positive of 4000 V, capillary voltage negative of 3500 V, and
negative and positive ion scanning modes from 50 to 1000 m/z. The
phenolic compounds were identified by comparing retention times of
unknown peaks to those of standard compounds.
2.4.5. Analysis of total phenolic content
Fifty mg of sample was extracted with ethanol–water (50:50, v/v) in
three steps (1, 0.5, 0.5 ml). After vortexing (5 min) and centrifugation
(6080 ×g for 5 min) in each stage, supernatants were collected in a
test tube. Combined extract was diluted 10 fold with the mixture of eth-
anol and water (50:50, v/v) prior to measurement.
The total phenolic content was determined according to the Folin–
Ciocalteu method with some modifications (Hoff & Singleton, 1977).
Extract (0.2 ml) was mixed with Folin–Ciocalteu reagent (0.8 ml) dilut-
ed with distilled water (1:10, v/v) and 20% aqueous Na2CO3 solution
(0.8 ml). After the mixture was allowed to stand in the dark for 2 h,
the tubes were centrifuged at 7155 ×g for 2 min and the absorbance
of supernatant was measured at 765 nm using UV–vis spectrophotom-
eter (Shimadzu, Kyoto, Japan). Standard calibration curve was prepared
at different concentrations of gallic acid (0–100 μg/ml) to determine
total phenolic content as mg of gallic acid equivalent (GAE) per gram
of sample.
2.4.6. Analysis of total antioxidant capacity
Fifty mg of sample was extracted with ethanol–water (50:50, v/v) in
three steps (1, 0.5, 0.5 ml). After vortexing (5 min) and centrifugation
(6080 ×g for 5 min) in each stage, supernatants were collected in a
test tube. Combined extract was diluted 10 fold with the mixture of eth-
anol and water (50:50, v/v) prior to measurement. Antioxidant activity
was determined using ABTS method. Stock solution of ABTS• + was pre-
pared by reacting 7 mM aqueous solution of ABTS with 2.45 mM potas-
sium persulfate and allowing the mixture to stand in the dark at room
temperature for 12–16 h before use. ABTS•+ working solution was ob-
tained by diluting the stock solution in water/ethanol mixture (50:50,
v/v) (Re et al., 1999). Extract (100 μl) was weighed into a centrifuge
tube and the reaction was started by adding 10 ml of ABTS working so-
lution. The mixture was stood in the dark for 28 min and the tube was
centrifuged at 9200 ×g for 2 min. After 30 min of reaction, the absor-
bance of the supernatant was measured at 734 nm by using UV–vis
spectrophotometer. The antioxidant activity of samples was calculated
by using standard calibration curve prepared at different concentrations
of Trolox (0–600 μg/ml) as mmol Trolox equivalent (TE) per gram of
sample.
2.5. Statistical analysis
The results were reported as mean ± standard deviations (S.D.).
Significant differences (p b 0.05) were evaluated by Duncan test after
4 K.S. Özdemir et al. / Food Research International xxx (2014) xxx–xxx

the analysis of variance (ANOVA), by using SPSS 17.0 statistical package. the pellicle contained less than 50% of the total antioxidants compared
Results of L*a*b* in samples before and after high shear homogenization to nuts with the pellicle (Blomhoff, Carlsen, Andersen, & Jacobs, 2006).
were compared by independent samples t-test. Colaric, Veberic, Solar, Hudina, and Stampar (2005) also showed that al-
though the skin of walnut (Juglans regia L.) contributed to the fruit weight
of only 5%, the phenolic contents of pellicle were quite high in compari-
3. Results and discussion son with kernel. According to Arcan and Yemenicioğlu (2009), the re-
moval of seed coat reduced the total antioxidant activity of hazelnuts at
3.1. Chemical characterization of hazelnut skin and its oil almost 36%. Similarly, it was reported by Schmitzer, Slatnar, Veberic,
Stampar, and Solar (2011) that skin removal negatively affected total
Table 1 gives basic chemical composition of hazelnut skin. Moisture phenolic content and antioxidant activity of hazelnuts. The other authors
(7.4%), protein (8.2%) and ash (1.7%) contents of hazelnut skin were also determined that hazelnut skin showed higher antioxidant activity
similar to those reported by Anil (2007) and Locatelli et al. (2010). It than other by-products in β-carotene–linoleate model system. Hazelnut
was found that dietary fiber was the main constituent of hazelnut skin skin extract exhibited the highest antioxidative activity by retaining
with its percentage contribution of 67.7%, of which 57.7% was insoluble β-carotene in the medium, followed by hazelnut hard shell, hazelnut
fiber. Montella, Coisson, Travaglia, Locatelli, Malfa, Martelli, et al. (2013) tree leaf, hazelnut green leafy cover, and hazelnut kernel (Shahidi et al.,
and Anil (2007) also remarked that hazelnut skin is a rich source of di- 2007).
etary fiber with the level of 58.3% and 64.2%, respectively. Due to reduc- Hazelnut skin oil was found to contain a unique amount of tocoph-
ing risk for developing coronary heart disease, hypertension, diabetes, erol vitamers. Total tocopherol content (sum of α-, β-, γ- and
obesity, and certain gastrointestinal diseases, high dietary fiber content δ-tocopherol) of oil was measured to be 2.77 μg/g oil (Table 1). This
of hazelnut skin has an importance in terms of health benefits (Lairon value is apparently higher compared to the oil extracted from hazelnut
et al., 2005; Liu et al., 1999; Montonen, Knekt, Jarvinen, Aromaa, & kernel, which was reported at 0.52 μg/g oil (Karabulut, Topcu, Yorulmaz,
Reunanen, 2003; Petruzziello, Iacopini, Bulajic, Shah, & Costamagna, Tekin, & Ozay, 2005). Moreover this amount is even higher than the
2006; Whelton et al., 2005). Montella, Coisson, Travaglia, Locatelli, total tocopherol content of wheat germ oil, which is known to be one
Bordiga, Meyrand, et al. (2013) characterized over thirty complex of the richest sources for tocopherols with the concentration of
free oligosaccharides, composed mainly of galacturonic acid and 2.57 μg/g oil (Schwartz, Ollilainen, Piironen, & Lampi, 2008). To make
N-acetylgalactosamine in hazelnut skin. Therefore, hazelnut skin a comparison it should be noted that commonly consumed vegetable
might be evaluated as a functional food ingredient in food formulations oils such as corn oil and sunflower oil were reported to contain 0.63
in spite of being a waste material of hazelnut industry. and 0.66 μg/g total tocopherols, respectively (Schwartz et al., 2008).
To date, some nut by-products have been investigated and remarked Among four tocopherol vitamers γ-tocopherol is the prominent one
as a source of natural antioxidants and phenolic compounds (Monagas with the concentration of 1.29 μg/g. It was followed by α, β and
et al., 2009; Salcedo, Lopez de Mishima, & Nazareno, 2010). In our δ-tocopherols with the concentrations of 1.25, 0.85 and 0.14 μg/g,
study, total phenolic content and antioxidant capacity of hazelnut skin respectively.
were found to be 233.7 mg GAE/g and 2.57 mmol TE/g, respectively. Tocopherols are known as good lipid soluble antioxidants present in
Monagas et al. (2009) reported that total phenolic content in the all vegetable oils in different quantities. They protect oils from oxidative
methanol/HCl extracts from roasted hazelnut skin was 107 mg GAE/g. deteriorations and show vitamin E activity in the human body
This difference might be related to various extraction conditions (Seppanen, Song, & Csallany, 2010). Hazelnut skin oil with its outstand-
and solvents. Total phenolic content of hazelnut skin was relatively ing tocopherol content could be used to fortify low tocopherol contain-
higher as compared to the other nut skins such as skin of almond ing oils, fats or foods to increase oxidative stability and vitamin E
(22.8 mg GAE/g), peanut (73.9 mg GAE/g) and walnut (101 mg GAE/g) activity. Along with high phenolic content, tocopherols contribute to
(Monagas et al., 2009; Salcedo et al., 2010). Similarly, total phenolic con- the antioxidant capacity of hazelnut skin. Thus hazelnut skin is an inter-
tent and antioxidant capacity of hazelnut skin were higher than those of esting coloring food ingredient with high phytochemical content.
pistachio skin, which were 116.32 mg GAE/g and 2.19 mmol TE/g, re- Oleic acid was found to be principle fatty acid of hazelnut skin oil
spectively (Tomaino et al., 2010). It was highlighted that nuts without with the percentage of 75.2 (Table 1). This value is quite close to the
data that reported the fatty acid composition of hazelnut kernel oil
(Cristofori, Ferramondo, Bertazza, & Bignami, 2008; Parcerisa,
Table 1
Richardson, Rafecas, Codony, & Boatella, 1998). The secondary fatty
Chemical composition of hazelnut skin and its oil.
acid of hazelnut skin oil was linoleic acid that was detected at the
Component Amount level of 16.2%. Saturated fatty acids of palmitic and stearic acid contents
Hazelnut skin of hazelnut skin oil were found to be 6.8 and 1.2%, respectively. Other
Moisture 7.4 ±0 0.3% fatty acids whose percentage was under 1% were not reported. These
Total dietary fibers results indicate that hazelnut skin oil is a rich source of oleic acid,
Soluble 10.0 ± 1.2%
which is a monounsaturated fatty acid (MUFA). It is well known
Insoluble 57.7 ± 1.9%
Proteins 8.2 ± 0.3% that consumption of MUFA rich oils such as olive and canola oil
Oil 14.5 ± 0.4%
Ash 1.7 ± 0.1% Table 2
Total phenolic content 233 ± 7 mg GAE/g Effect of pass cycles and pressure applied during high shear homogenization on the
Total antioxidant capacity 2.57 ± 0.12 mmol TE/g particle size distribution of fine hazelnut skin powders.
Hazelnut skin oil
Fatty acid composition (%) Pass cycle Mean particle size, μm
C16:0 palmitic acid 6.8 ± 0.01%
10 ksi 20 ksi 30 ksi
C18:0 stearic acid 1.2 ± 0.01%
C18:1 oleic acid 75.2 ± 0.06% 0 (feed) 107.7 ± 6.7a 107.7 ± 6.7a 107.7 ± 6.7a
C18:2 linoleic acid 16.2 ± 0.02% 1 32.9 ± 0.1b 36.9 ± 1.4b 17.9 ± 0.1b
Total tocopherols 2.77 ± 0.02 μg/g 3 25.4 ± 0.3c 23.9 ± 0.7c 32.4 ± 5.1c
α-Tocopherol 1.25 ± 0.02 μg/g 5 22.8 ± 0.4c 26.1 ± 0.4c 42.8 ± 3.8d
β-Tocopherol 0.85 ± 0.01 μg/g 10 22.7 ± 0.7c 50.2 ± 1.2d 52.8 ± 3.5e
γ-Tocopherol 1.29 ± 0.01 μg/g
The results are given as mean ± S.D. Different letters within the same column indicates
δ-Tocopherol 0.14 ± 0.01 μg/g
statistical significance (p b 0.05).

Please cite this article as: Özdemir, K.S., et al., Hazelnut skin powder: A new brown colored functional ingredient, Food Research International
(2014), http://dx.doi.org/10.1016/j.foodres.2014.01.060
 K.S. Özdemir et al. / Food Research International xxx (2014) xxx–xxx 5

8
b When the number of homogenization passes increased, particle size
7 continued to decrease and began to increase afterward. This increase
6 a can be related to the tendency of particles to re-coalesce at these pres-
sures (10–30 ksi) and pass (1–10) conditions. Similar circumstance
Volume (%)

5
4
3 sion droplet size (Jafari, He, & Bhandari, 2006; Jafari, He, & Bhandari,
2 2007; Lobo & Svereika, 2003). It was also reported that the smaller par-
1
0
0.01 0.1 1 10 100 1000 10000
Particle size (µm)
Fig. 2. Particle size distribution of hazelnut skin powders. (a) Coarse powder (low shear
homogenized), (b) fine powder (high shear homogenized at 30 kpsi with single pass
cycle).
(Gillingham, Harris-Janz, & Jones, 2011) has positive effects on human
health. Besides, compared to polyunsaturated fatty acids, MUFA rich
oils have better oxidative stability.
3.2. Physical and chemical characterizations of coarse and fine hazelnut
skin powders
3.2.1. Physical characterization
Table 2 gives the impact of pass cycles on D(0.5) of fine hazelnut skin
powders at different pressures. High shear homogenization was an effi-
cient technique for producing low micron sized particles compared with
low shear homogenizers. The D(0.5) of the coarse hazelnut skin powder
(feed) which was pre-homogenized by using a low shear mixer was
107.7 μm. There was a sharp decrease in the D(0.5) of samples after
one pass through the high shear homogenizer at all pressures studied.
D(0.5) of samples dropped from 107.7 μm to 32.9 μm, 36.9 μm and 17.9
μm at pressures of 10, 20 and 30 ksi, respectively. Also, after homogeni-
zation the distribution profile of particle size shifted left and narrowed
(a typical Gaussian distribution), indicating that the particle size of the
hazelnut skin fibers decreased. When pressure increased at constant
pass, the distribution profile became narrower and more homogenous
as shown in Fig. 2.
has been previously reported in emulsion systems as “over-processing”
which is a re-coalescence of emulsion droplets and an increase in emul-
ticle causes the greater aggregation (Tu et al., 2013). Particles began to
re-coalesce at different passes for various pressures. For instance,
D(0.5) began to increase after 5 pass at 20 ksi and 3 pass at 30 ksi.
Fig. 3 indicates scanning electron microscopy (SEM) images of fine
hazelnut skin powder (high shear homogenized at 10 kpsi with a single
pass cycle) and coarse hazelnut skin powder. Particle size reduction
could also be seen from these images of the samples. Coarse powder
had a relatively plainer structure. However, after high shear homogeni-
zation, the structure was damaged and changed into smaller fragments.
It was also reported that the structure of the complexes could be broken
into smaller fragments after high-shear homogenization (Chen et al.,
2012; Hu, Nie, & Xie, 2013). Chen et al. (2012) reported that the original
flake-like structure of pectin was totally changed into smaller chips.
Changes of hazelnut skin powder color with high shear homogeniza-
tion were investigated using the L* (lightness), a* (redness) and b*
(yellowness) and ΔE (color difference) parameters. The L*, a*and b*
values of coarse hazelnut skin powder were 55.8, 8.4 and 11.1 respec-
tively. To calculate ΔE, color values of coarse powder were taken as
the reference and ΔE was found to be 2.54 ± 0.93. After high shear ho-
mogenization, values of L*, a* and b* were 57.9, 9.2 and 12.3 respectively
and increased significantly (p b 0.05). Due to increasing redness param-
eter with high shear homogenization, brown color intensity of hazelnut
skin powder could be improved. In general, high-shear homogenization
treatment of hazelnut skin produced brighter powder with more red-
ness and yellowness.
3.2.2. Chemical characterization
The ABTS radical scavenging activity and total phenolic content of
coarse and fine hazelnut skin powders were given in Table 3. The anti-
oxidant activity of coarse powder was found at 2.57 ± 0.12 mmol TE/g.
The antioxidant activity of the fine powders did not change after the
high shear homogenization treatment at 10 ksi and 30 ksi. At 20 ksi,

Fig. 3. Scanning electron microscopy images of hazelnut skin powders (scale bar 30 μm, 2500× magnification). (a) Coarse powder (low shear homogenized), (b) fine powder (high shear
homogenized at 10 kpsi with single pass cycle).

Please cite this article as: Özdemir, K.S., et al., Hazelnut skin powder: A new brown colored functional ingredient, Food Research International
(2014), http://dx.doi.org/10.1016/j.foodres.2014.01.060
6 K.S. Özdemir et al. / Food Research International xxx (2014) xxx–xxx

Table 3
Effect of pass cycles and pressure applied during high shear homogenization on the total antioxidant capacity and total phenolic content of fine hazelnut skin powders.

Pass cycle Total antioxidant activity, mmol TE/g Total phenolic content, mg GAE/g

10 ksi 20 ksi 30 ksi 10 ksi 20 ksi 30 ksi

a a a a a
0 (feed) 2.57 ± 0.12 2.57 ± 0.12 2.57 ± 0.12 232.6 ± 7 232.6 ± 7 232.6 ± 7a
1 2.2 ± 0.26a 2.0 ± 0.01b 267 ± 0.18a 189.5 ± 7.9bc 227 ± 9ab 191 ± 13b
3 2.2 ± 0.11a 1.9 ± 0.13b 2.7 ± 0.01a 199.0 ± 4.1b 213 ± 3b 198 ± 14b
5 2.2 ± 0.09a 2.0 ± 0.14b 2.9 ± 0.26a 202.7 ± 12.7b 218 ± 2ab 215 ± 13ab
10 2.2 ± 0.18a 2.4 ± 0.03a 2.6 ± 0.46a 176.5 ± 1.0c 219 ± 5ab 210 ± 13ab

The results are given as mean ± S.D. Different letters within the same column indicates statistical significance (p b 0.05). Initial total antioxidant capacity and total phenolic content of the
coarse powder are 2.57 ± 0.12 mmol TE/g and 233 ± 7 mg GAE/g, respectively.

antioxidant activity was decreased significantly after 1 pass but it 4. Conclusion

remained constant until 10 passes. According to the results, increasing
the pass number did not affect the antioxidant activity significantly
(p b 0.05). A similar trend was observed in the results of total phenolic
content. Total phenolic content of coarse powder was found at 232.6 ±
7 mg GAE/g. After high shear homogenization there was a reduction in
the total phenolic content but an increase in the pass number (from 1
pass to 10 pass) did not affect it significantly.
Hazelnut skin powders were found to contain relatively large
amounts of free soluble phenolic compounds (Table 4), while soluble
conjugated and insoluble bound phenolic compounds were below the
limit of quantification. Catechin, epicatechin, epicatechin gallate,
gallocatechin, epigallocatechin gallate, and gallic acid were detected in
soluble free fraction. Gallic acid was the most abundant phenolic acid,
with a concentration range of 49.7–80.3 mg/100 g. Shahidi et al.
(2007) reported ferulic and sinapic acids in hazelnut skin differently
from the results of this study, but similarly, gallic acid was most
abundant in hazelnut skin. Moreover, gallic acid was determined most
abundant phenolic acid among the free and esterified phenolic acids
of hazelnut green leafy cover (Alasalvar, Karamac, Amarowicz, &
Shahidi, 2006).
Flavan-3-ols are abundant flavonoids occurring as monomers and as
oligomeric and polymeric forms (also called proanthocyanidins).
Monagas et al. (2009) determined flavon-3-ol composition of hazelnut
skin and found that total monomers accounted for 90%. Del Rio et al.
(2011) also identified the hazelnut skin polyphenolic composition and
found that the main polyphenolic subclass, comprised monomeric and
oligomeric flavan-3-ols, which accounted for more than 95% of total poly-
phenols. According to their work, at least nine B-type dimers of
procyanidins were identified in the hazelnut skin. In our study, catechin,
epicatechin, epicatechin gallate, gallocatechin, and epigallocatechin
gallate known as monomeric flavan-3-ols were detected in soluble free
fraction. The concentration of catechin (49.9–67.8 mg/100 g) was much
higher than other flavan-3-ols in the samples. In a previous study,
(+)-catechin was found to be more abundant than (−)-epicatechin in
roasted hazelnut skins (Monagas et al., 2009). In general, increasing pres-
sure up to 20 ksi during high shear homogenization did not affect the
concentrations of phenolic compounds. However, there were significant
reductions (p b 0.05) in the concentrations of epicatechin and gallic
acid when pressure was increased to 30 ksi.
In this study, the effect of high-shear homogenization technique was
investigated to produce low-micron sized hazelnut skin powders. The
results from laser scattering measurements indicated a significant de-
crease in particle size after homogenization. The particle size decreases
when a higher shear rate was applied during processing. Then, cluster-
ing of stable particle was observed at high shear rates and increased
pass cycles. Additionally, fine hazelnut skin powders exhibited lighter
and browner color intensity compared to the coarse hazelnut skin pow-
der. According to the results, increase in the pass number did not affect
the antioxidant activity significantly (p b 0.05). This similar trend was
observed in the results of total phenolic content. Also the results sug-
gested that the high shear homogenization technology has no signifi-
cant effect on the polyphenol's compositions of hazelnut skins. But
generally increasing pressure up to the 30 ksi was not effective on
polyphenols.
From a practical point of view, a single pass high shear homogeniza-
tion at 10 ksi is appropriate for obtaining low-micron sized hazelnut
skin powder. Hence, the findings of this study may pave a way for the
utilization of a low-valued industrial by-product to be a natural coloring
agent with a rich source of phenolic compounds and dietary fibers in
functional food formulations. The results obtained from chemical com-
position analyses of hazelnut skin oil indicated that this oil is very rich
in health-promoting tocopherols and oleic acid. Further studies are
needed to explore the effects of low-micron sized hazelnut skin pow-
ders and hazelnut skin oil in different food formulations.
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Table 4
Effect of pressure on the composition of individual phenolic compounds in fine hazelnut skin powders obtained by a single pass high shear homogenization at different pressures.

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Please cite this article as: Özdemir, K.S., et al., Hazelnut skin powder: A new brown colored functional ingredient, Food Research International
(2014), http://dx.doi.org/10.1016/j.foodres.2014.01.060
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