Chemical characterization of the lipophilic fraction of giant reed

Industrial Crops and Products 26 (2007) 229–236
Chemical characterization of the lipophilic fraction of giant reed
(Arundo donax) fibres used for pulp and paper manufacturing
Dora Coelho a,b , Gisela Marques a , Ana Gutiérrez a ,
Armando J.D. Silvestre b , José C. del Rı́o a,∗
a
Instituto de Recursos Naturales y Agrobiologı́a de Sevilla, Consejo Superior de Investigaciones Cientı́ﬁcas,
P.O. Box 1052, 41080 Seville, Spain
b CiCECO and Department of Chemistry, University of Aveiro,
3810-193 Aveiro, Portugal
Received 7 February 2007; received in revised form 27 March 2007; accepted 2 April 2007
Abstract
The chemical composition of lipophilic extractives from Arundo donax stems (including nodes and internodes), used for pulp
and papermaking, was studied. The lipid fraction was extracted with acetone and redissolved in chloroform, and then fractionated
by solid-phase extraction (SPE) on aminopropyl-phase cartridges into four different fractions of increasing polarity. The total lipid
extract and the resulting fractions were analysed by gas chromatography and gas chromatography/mass spectrometry, using shortand medium-length high-temperature capillary columns, respectively. The main compounds identified in the fibres included series
of long-chain n-fatty acids, n-alkanes, n-aldehydes, n-alcohols, monoglycerides, free and esterified sterols and triterpenols, steryl
glucosides, steroid hydrocarbons and steroid and triterpenoid ketones. Minor amounts of other compounds such as diglycerides,
waxes and tocopherols were also identified among the lipids of A. donax.
© 2007 Elsevier B.V. All rights reserved.
Keywords: Arundo donax; Lipophilic extractives; Pitch; Fatty acids; Sterols; Steryl glucosides; GC; GC/MS
1. Introduction
In the last decades, fast growing plants have received
particular attention as alternative sources of cellulose
fibres (van Dam et al., 1994; Moore, 1996). These nonwood plants are the common fibre source for paper
pulp production in developing countries where wood
fibres are not available. In the developed world, although
wood is still by far the main raw material for pulp and
∗ Corresponding author. Tel.: +34 95 462 4711;
fax: +34 95 462 4002.
E-mail address: delrio@irnase.csic.es (J.C. del Rı́o).
0926-6690/$ – see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.indcrop.2007.04.001
paper manufacture, a market exists for high-value-added
papers from these fibres. Arundo donax L. (giant reed)
is a widely distributed naturally growing perennial rhizomatous grass with a segmented tubular structure like
bamboo (Seca et al., 2000), which has been considered as one of the promising non-wood plants for pulp
and paper industry (Shatalov and Pereira, 2002). The
easy adaptability to different ecological conditions, the
annual harvesting period and the high biomass productivity (32–37 t (year ha)−1 of dry biomass) reached by
intensive cultivation (Vecchiet et al., 1996), combined
with appropriate chemical composition (Shatalov et al.,
2001), make A. donax very attractive as an alternative
source of fibres (Shatalov and Pereira, 2005).
230
D. Coelho et al. / Industrial Crops and Products 26 (2007) 229–236
To improve the utilisation of A. donax fibres, it is necessary to broaden the knowledge of structural features of
its components. Previous chemical research on A. donax
includes chemical composition, general features of
macromolecular components (Pascoal Neto et al., 1997)
and structures of isolated hemicelluloses (Driss et al.,
1973; Joseleau and Barnoud, 1974, 1975, 1976). A few
studies on the lignin composition (Joseleau and Barnoud,
1976; Joseleau et al., 1976; Faix et al., 1989) showed that
it is composed of guaiacyl- and syringyl-propane units
with minor amounts of p-hydroxyphenylpropane units
(Faix et al., 1989) and associated with phenolic acids
(Tai et al., 1987). However, until now no studies about
the composition of A. donax lipophilic fraction have been
performed.
The amount and composition of lipophilic extractives
is an important parameter in wood processing for pulp
and paper production and it is dependent on factors such
as the plant species, age, and growth location. The different lipid classes have different chemical behaviour
during pulping and bleaching (Gutiérrez and del Rı́o,
2003; Freire et al., 2005). The lipophilic extractives are
also responsible for the formation of sticky deposits on
the machinery, giving rise to dark spots in bleached pulp
and paper, the so-called pitch, both with negative economic impact on pulp and paper industry (del Rı́o et
al., 1998, 2000; Gutiérrez et al., 2004; Gutiérrez and
del Rı́o, 2005; Silvestre et al., 1999). The accumulation
of lipophilic compounds leads also to higher chemicals
consumption during pulping and bleaching and therefore
increasing production costs. On the other hand, extractives or their derivatives, might contribute to the toxicity
of paper pulp effluents and products (McCubbin and
Folke, 1995; Rigol et al., 2003). The detailed identification of such lipophilic components is therefore an
important step in the study of the behaviour and fate of
extractives during pulp and paper production and consequently in the search for new solutions to control pitch
deposition as well as to decrease effluent toxicity.
In the present paper, the chemical composition of the
lipophilic extractives from A. donax fibres was studied.
Gas chromatography (GC) and GC/mass spectrometry
(GC/MS) using, respectively, short- and medium-length
high-temperature capillary columns with thin films, that
enable elution and separation of high-molecular-mass
lipids such as waxes, steryl esters and triglycerides,
are employed. For a more detailed characterization
of the different homologous series and other minor
compounds, the extract was fractionated by a simple
solid-phase extraction (SPE) method using aminopropyl
phase cartridges, as described previously (Gutiérrez et
al., 1998, 2004).
2. Experimental
2.1. Samples
Samples of A. donax L. reed stems (including nodes
and internodes) were supplied by the University of
Huelva, Spain. The samples were air-dried and milled
using a knife mill (Janke and Kunkel, Analysenmühle).
For the isolation of lipids, the milled samples were
Soxhlet extracted with acetone for 8 h. The lipophilic
extractives were obtained by redissolving the dried acetone extract in chloroform and evaporated to dryness
under nitrogen.
2.2. Solid phase extraction (SPE) fractionation
The chloroform extracts (5–20 mg) were fractionated
by a SPE procedure in aminopropyl phase cartridges
(500 mg) from Waters (Division of Millipore, Milford,
MA, USA), as already described (Gutiérrez et al., 1998,
2004). Briefly, the dried extract was taken up in a minimal volume (<0.5 mL) of hexane:chloroform (4:1) and
loaded into the cartridge column previously conditioned
with hexane (4 mL). The cartridge was loaded and eluted
by gravity. The column was first eluted with 8 mL of hexane and subsequently with 6 mL of hexane:chloroform
(5:1), then with 10 mL of chloroform and finally with
10 mL of diethyl ether:acetic acid (98:2). Each isolated
fraction was dried under nitrogen.
2.3. GC and GC/MS analyses
For identification and quantification, the total extracts
and the SPE fractions were analysed by GC and GC/MS.
For GC analysis, a Hewlett-Packard HP 5890 gas chromatograph equipped with split–splitless injector and
a flame ionization detector (FID) system was used
(Hewlett-Packard, Hoofddorp, Netherlands). The injector and detector temperatures were set at 300 and 350 ◦ C,
respectively. Duplicate samples (1 ␮L) were injected
in the splitless mode. Helium was used as the carrier
gas. The capillary column used was a 5 m × 0.25 mm
i.d., 0.1 ␮m film thickness, high-temperature, polyimidecoated fused silica tubing DB-5HT from J&W Scientific
(Folsom, CA), especially processed for use at 400 ◦ C.
The oven was temperature programmed from 100 ◦ C
(1 min) to 350 ◦ C (3 min) at 15 ◦ C min−1 . Peaks were
quantified by area and a mixture of standards (tetracosane, hexadecanoic acid, ␤-sitosterol, cholesteryl
oleate and triheptadecanoin) was used for quantitation.
The data from the two replicates was averaged.
D. Coelho et al. / Industrial Crops and Products 26 (2007) 229–236
The GC/MS analysis were performed on a Varian
Star 3400 gas chromatograph (Varian, Walnut Creek,
CA) coupled with an ion-trap detector (Varian Saturn)
equipped with a high-temperature capillary column (DB5HT, 15 m × 0.25 mm i.d., 0.1 ␮m film thickness; J&W).
Helium was used as carrier gas at a rate of 2 ml min−1 .
The oven was heated from 120 ◦ C (1 min) to 380 ◦ C
(5 min) at 10 ◦ C min−1 . The temperature of the injector
during the injection was 120 ◦ C, and 0.1 min after injection was programmed to 380 ◦ C at a rate of 200 ◦ C/min
and held for 10 min. The temperature of the transfer line
was set at 300 ◦ C. Bis(trimethylsilyl)trifluoroacetamide
(BSTFA) silylation was used when required. Compounds were identified by comparing their mass spectra
with mass spectra in Wiley and NIST libraries, by mass
fragmentography, and, when possible, by comparison
with authentic standards.
3. Results and discussion
The total acetone extract from A. donax fibres
accounted for 1.56% of total fibre weight. The lipophilic
– chloroform soluble – compounds represented 0.62%,
while the remaining 0.94% corresponded to polar compounds non-soluble in chloroform. The lipid extracts
were analyzed by GC and GC/MS according to the
method previously described (Gutiérrez et al., 1998,
2004). The GC/MS chromatogram of the A. donax
fibres extract, as trimethylsilyl (TMS) derivatives, is
shown in Fig. 1. For a better characterization of the
compounds present in the lipid extracts, these were sub-
231
sequently fractionated by SPE in aminopropyl-phase
cartridges into four major fractions of increasing polarity. The chromatograms of the different SPE fractions
are shown in Fig. 2. The first fraction (A), eluted
with hexane, was enriched in steryl esters, waxes and
hydrocarbons. The second fraction (B), eluted with hexane:chloroform (5:1), contained steroid ketones. The
third fraction (C), eluted with chloroform, contained
sterols, fatty alcohols and mono- and diglycerides. A
final fraction (D) enriched in free fatty acids was eluted
with diethyl ether–acetic acid (98:2). The identities and
abundances of the main compounds identified are listed
in Table 1. The most predominant lipid classes identified among the A. donax lipid extracts were series
of n-fatty acids (41% of total lipids identified), sterols
(19%), monoglycerides (13%), fatty alcohols (7%) and
steryl glucosides (6%). Minor amounts of alkanes, aldehydes, tocopherols, steroid hydrocarbons, steroid and
triterpenoid ketones and steryl/triterpenyl esters, were
also present in these fibres. The structures of main and
representative compounds are shown in Fig. 3.
The series of free fatty acids were identified in
A. donax fibres ranging from tetradecanoic (C14 ) to
dotriacontanoic (C32 ) acids, with strong even-overodd carbon atom predominance. Hexadecanoic acid
(palmitic acid, I) was the most abundant fatty acid, however a bimodal distribution, with a second maximum for
octacosanoic acid (C28 ) was observed. The unsaturated
9-octadecenoic (oleic acid, II) and 9,12-octadecadienoic
(linoleic acid, III) acids were also present in important
amounts. The series of n-alkanes was also identified in
Fig. 1. GC/MS chromatogram of the derivatized (TMS) chloroform extract of Arundo donax fibres. FA: fatty acids; MG: monoglycerides; CG:
campesteryl 3␤-d-glucopyranoside; StG: stigmasteryl 3␤-d-glucopyranoside; SG: sitosteryl 3␤-d-glucopyranoside.
232
D. Coelho et al. / Industrial Crops and Products 26 (2007) 229–236
Fig. 2. GC/MS chromatograms of the different SPE fractions isolated from the A. donax fibres extracts. Fraction A, eluted with 8 mL of hexane;
fraction B, eluted with 6 mL of hexane:chloroform (5:1); fraction C, eluted with 10 mL of chloroform; and fraction D, eluted with 10 mL diethyl
ether:acetic acid (98:2). FA: fatty acids; AK: n-alkanes.
the A. donax fibre ranging from docosane (C22 ) to tritriacontane (C33 ), with a strong odd-over-even carbon
atom number predominance, and nonacosane (IV) being
the most predominant homolog. n-Fatty alcohols ranging from hexacosanol (C26 ) to dotriacontanol (C32 ) were
present in the A. donax extracts with the presence of only
the even carbon atom number homologues, triacontanol
(V) being the most abundant. Significant amounts of a
series of n-aldehydes ranging from hexacosanal (C26 ) to
triacontanal (C30 ) were identified in the A. donax fibres
D. Coelho et al. / Industrial Crops and Products 26 (2007) 229–236
233
Table 1
Chemical composition of lipophilic extractives in Arundo donax reed (mg/kg of fibre)
Compound
Mass Fragments
MW
Amount
n-Alkanes
n-Docosane
n-Tricosane
n-Tetracosane
n-Pentacosane
n-Hexacosane
n-Heptacosane
n-Octacosane
n-Nonacosane
n-Triacontane
n-Hentriacontane
n-Dotriacontane
n-Tritriacontane
57/71/85/310
57/71/85/324
57/71/85/338
57/71/85/352
57/71/85/366
57/71/85/380
57/71/85/394
57/71/85/408
57/71/85/422
57/71/85/436
57/71/85/450
57/71/85/464
310
324
338
352
366
380
394
408
422
436
450
464
77.9
0.5
0.2
0.6
6.3
3.9
15.8
6.7
37.0
0.8
5.4
0.3
0.4
Steroid hydrocarbons
Ergostatriene
Ergostadiene
Estigmastadiene
Estigmasta-3,5,22-triene
Estigmasta-3,5-diene
135/143/380
81/147/367/382
81/147/381/396
135/143/394
81/147/381/396
380
382
396
394
396
127.4
14.5
9.3
8.4
49.2
46.0
Fatty acids
n-Tetradecanoic acid
n-Pentadecanoic acid
n-Hexadecanoic acid
n-Heptadecanoic acid
9,12-Octadecadienoic acid
9-Octadecanoic acid
n-Octadecanoic acid
n-Nonadecanoic acid
n-Eicosanoic acid
n-Heneicosanoic acid
n-Docosanoic acid
n-Tricosanoic acid
n-Tetracosanoic acid
n-Pentacosanoic acid
n-Hexacosanoic acid
n-Heptacosanoic acid
n-Octacosanoic acid
n-Nonacosanoic acid
n-Triacontanoic acid
n-Hentriacontanoic acid
n-Dotriacontanoic acid
73/117/132/145/285/300a
73/117/132/145/299/314a
60/73/129/256
73/117/132/145/327/342a
67/81/280
55/69/264
60/73/129/284
73/117/132/145/355/370a
60/73/129/312
55/69/129/326
60/73/129/340
60/73/129/354
60/73/129/368
60/73/129/382
73/117/132/145/453/468a
73/117/132/145/467/482
73/117/132/145/482/496a
73/117/132/145/495/510a
73/117/132/145/509/525a
73/117/132/145/523/538
73/132/145/117/537/552a
300a
314a
256
342a
280
282
284
370a
312
326
340
354
368
382
468a
482a
496a
510a
525a
538a
552a
1137.7
3.5
1.8
276.3
10.0
30.0
55.7
73.6
3.1
50.0
3.3
35.7
25.3
55.7
33.5
144.1
14.3
134.9
53.9
109.9
6.2
16.9
Fatty alcohols
n-Hexacosanol
n-Octacosanol
n-Triacontanol
n-Dotriacontanol
75/103/439a
75/103/467a
75/103/495a
75/103/523a
454a
482a
510a
538a
194.3
33.4
54.9
57.7
48.3
Aldehydes
n-Hexacosanal
n-Octacosanal
n-Triacontanal
82/96/362
82/96/390
82/96/418
380
408
436
81.6
10.4
22.9
48.3
Sterols/triterpenols
Campesterol
Stigmasterol
␤-Sitosterol
Stigmastanol
55/145/213/382/400
55/81/255/394/412
145/213/396/414
215/416
400
412
414
416
528.1
90.6
46.4
281.0
71.9
234
D. Coelho et al. / Industrial Crops and Products 26 (2007) 229–236
Table 1 (Continued )
Compound
Mass Fragments
MW
Amount
7-oxo-Sitosterol
␤-Amyrin
␣-Amyrin
135/161/187/396/428
189/203/218/409/426
189/203/218/409/426
428
426
426
6.5
8.2
23.5
Tocopherol
␤-Tocopherol
␣-Tocopherol
151/416
165/430
416
430
17.7
6.8
10.9
Triterpenoid and steroid ketones
␤-Amyrenone
␣-Amyrenone
Cycloartenone
Stigmasta-3,5-dien-7-one
Stigmast-4-en-3-one
Stigmast-4-en-3,6-dione
Stigmastane-3,6-dione
189/203/218/409/424
189/203/218/409/424
189/205/313/409/424
174/269/410
124/229/412
137/398/408/411/426
245/287/428
424
424
424
410
412
426
428
43.9
10.2
5.9
14.2
3.2
4.6
3.6
2.5
Steryl/triterpenyl esters
Sitosteryl ester
␤-Amyrinyl ester
␣-Amyrinyl ester
147/381/397
189/203/218
189/203/218
–
–
–
68.1
16.1
14.0
38.0
Steryl glucosides
Campesteryl 3-␤-d-glucopyranoside
Stigmasteryl 3-␤-d-glucopyranoside
Sitosteryl 3-␤-d-glucopyranoside
204/217/361/383a
204/217/361/395a
204/217/361/397a
850a
862a
864a
151.6
30.6
8.0
113.0
Monoglyceride
2,3-Dihydroxypropyl tetradecanoate
2,3-Dihydroxypropyl hexadecanoate
2,3-Dihydroxypropyl octadecanoate
2,3-Dihydroxypropyl eicosanoate
2,3-Dihydroxypropyl docosanoate
2,3-Dihydroxypropyl tetracosanoate
2,3-Dihydroxypropyl hexacosanoate
73/103/129/147/343/431a
73/103/129/147/371/459a
73/103/129/147/399/487a
73/103/129/147/427/515a
73/103/129/147/455/543a
73/103/129/147/483/571a
73/103/129/147/511/599a
446a
474a
502a
530a
558a
586a
614a
367.5
5.5
94.2
86.6
35.1
43.0
46.9
56.2
Diglycerides
Dipalmitin, 1,2-(P2)
Dipalmitin, 1,3-(P2)
Palmitoylstearin (PS)
Distearin, 1,2- and 1,3-(S2)
57/129/313/386/625a
57/129/314/371/385/625a
57/129/314/372/399/579a
57/129/342/399/607a
640a
640a
668a
696a
47.6
7.8
12.1
16.8
10.9
Each value is the average of two extractions with variation coefficients within 0.1–4.5%.
a As TMSi ether derivates; bold mass fragments indicate base peaks.
with triacontanal (VI) predominating. Monoglycerides
were also present in high amounts in A. donax fibres.
The series of monoglycerides was identified in the range
from C14 to C26 , with maximum for monopalmitin, C16
(VII).
Steroids and triterpenoids, including free sterols,
steryl esters, steryl glucosides, steroid ketones and
hydrocarbons are among the most predominant compounds in the lipophilic extract of A. donax fibre. Free
sterols were the major compound class among steroids
and triterpenoids, sitosterol (VIII) being the main
sterol present. Other sterols, such as campesterol (IX),
stigmasterol (X), stigmastanol (XI) and the oxidized 7oxositosterol, were also present. Steryl esters were also
present in A. donax extract, although in low amounts.
The complete identification of the individual steryl esters
by GC/MS was not possible since they only show fragments arising from the sterol moiety by electro-impact
MS and rarely give detectable molecular ions (Lusby et
al., 1984; Evershed et al., 1989). By monitoring the ions
corresponding to the different sterol moieties in the SPE
fraction enriched in steryl esters, it was possible to identify series of sitosterol as well as ␣- and ␤-amyrin esters.
Steryl glucosides, such as campesteryl, stigmasteryl and
sitosteryl ␤-d-glucopyranosides (XII), were identified
in significant amounts, the latter being the most predominant. The identification of steryl glucosides was
accomplished (after BSTFA derivatization of the lipid
D. Coelho et al. / Industrial Crops and Products 26 (2007) 229–236
235
Fig. 3. Structures of the main lipophilic compounds present in A. donax fibres. (I) palmitic acid, (II) oleic acid, (III) linoleic acid, (IV) nonacosane,
(V) triacontanol, (VI) triacontanal, (VII) monopalmitin, (VIII) ␤-sitosterol, (IX) campesterol, (X) stigmasterol, (XI) stigmastanol, (XII) sitosteryl
3␤-d-glucopyranoside, (XIII) ␣-amyrin, (XIV) ␤-amyrin, (XV) stigmasta-3,5-diene, (XVI) stigmasta-3,5,7-triene, (XVII) ␤-amyrenone, (XVIII)
␣-amyrenone, (XIX) cycloartenone, (XX) stigmasta-3,5-dien-7-one, (XXI) stigmast-4-en-3-one and (XXII) stigmasta-3,6-dione.
extract) by comparison with the mass spectra and relative retention times of authentic standards (Gutiérrez and
del Rı́o, 2001). Among triterpenols, ␣-amyrin (XIII)
and ␤-amyrin (XIV) occurred in free and esterified
form, with the latest being detected in low amounts.
Finally, several steroid hydrocarbons, such as stigmasta-
3,5-diene (XV) and stigmasta-3,5,7-triene (XVI) and
triterpenoid and steroid ketones, such as ␤-amyrenone
(XVII), ␣-amyrenone (XVIII), cycloartenone (XIX),
stigmasta-3,5-dien-7-one (XX), stigmast-4-en-3-one
(XXI) and stigmasta-3,6-dione (XXII), were also
identified.
236
D. Coelho et al. / Industrial Crops and Products 26 (2007) 229–236
The different lipid classes present in A. donax fibres
will have different behavior during pulping and bleaching and therefore the problematic of pitch will be
different depending the type of pulping (i.e. mechanical
and chemical) and bleaching (ECF and TCF) processes.
The knowledge of the chemical composition of the
lipophilic components of A. donax fibres shown here will
assist to predict pitch problems during pulp and papermaking of this fibre and to establish appropriate methods
for their control.
Acknowledgements
This study has been funded by the Spanish project
AGL2005-01748. GM thanks the Spanish Ministry of
Education and Science for a FPI fellowship. We thank
M.J. Diaz (University of Huelva) for the Arundo donax
fibres.
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