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Section of Lecce, Italy;2John Innes Centre, Norwich, UK Plant lipoxygenases LOXs are a class of dioxygenases which display diverse functions in several physiological processes such as gr

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Biochemical and molecular characterization of hazelnut

Angelo Santino1, Angelo De Paolis1, Antonia Gallo1,*, Angela Quarta1, Rod Casey2and Giovanni Mita1

1

Institute of Sciences of Food Production C.N.R Section of Lecce, Italy;2John Innes Centre, Norwich, UK

Plant lipoxygenases (LOXs) are a class of dioxygenases

which display diverse functions in several physiological

processes such as growth, development and response to

biotic and abiotic stresses.Even though LOXs have been

characterized from several plant species, the physiological

role of seed LOXs is still unclear.With the aim to better

clarify the occurrence of LOXs and their influence on

hazelnut seed quality, we carried out the biochemical and

molecular characterization of the main LOX isoforms

expressed during seed development.A genomic clone

con-taining a complete LOX gene was isolated and fully

char-acterized.The 9887 bp sequence reported contains an open

reading frame of 5334 bp encoding a putative polypeptide of

99 kDa.Semiquantitative RT-PCR carried out from RNAs

extracted from seeds at different maturation stages showed

that LOXs are mainly expressed at early developmental

stages.These results were confirmed by LOX activity assays

Biochemical characterization of the reaction products of the hazelnut LOX indicated that it is a 9-LOX.Two cDNAs were isolated by RT-PCR carried out on total RNA from immature hazelnut seeds.Sequence analysis indicated that the two cDNAs are highly homologous (91.9% degree of identity) and one of these corresponded exactly to the genomic clone.The deduced amino acid sequences of the hazelnut LOXs showed that they are closely related to

a previously reported almond LOX (79.5% identity) and, to

a lesser extent, to some LOXs involved in plant responses

to pathogens (cotton and tobacco LOXs, 75.5 and 74.6% identity, respectively).The physiological role of hazelnut LOXs and their role in influencing seed quality are also discussed

Keywords: Corylus avellana; hazelnut; lipoxygenases; seed quality

Lipoxygenases (LOX, EC 1.13.11.12) are a class of

widespread dioxygenases that catalyze the addition of

oxygen to polyunsaturated fatty acids containing a

cis,cis-1,4-pentadiene structure.The hydroperoxides produced by

the LOX reaction are the starting point for a series of

other enzymatic reactions which lead to the synthesis of a

group of biologically active compounds collectively named

oxylipins.In animal cells, the LOX pathway has been

extensively studied as it is responsible for the synthesis of

leukotrienes and lipoxins belonging to the eicosanoid

family which are involved in many physiological processes

[1].In plants the biosynthesis of phytooxylipins is initi-ated by the oxygen insertion at C-9 or C-13 of linoleic (C18 : 2) or linolenic acids (C18 : 3).For this reason plant LOXs are commonly referred as 9-LOXs or 13-LOXs Both 9- or 13-hydroperoxides are further converted to different compounds through the action of the other enzymes belonging to different branches of the LOX pathway (hydroperoxide lyase, allene oxide synthase, divinyl ether synthase, reductase, peroxygenase).At the end of these enzymatic reactions the molecules synthesized display a wide variety of physiological roles in plant development and response to biotic and abiotic stresses.In this context lipoxygenases, providing the substrates for the activity of all the enzymes located downstream on the pathway, have a primary role in the biosynthesis of phytooxylipins and can affect their availability inside the plant cell.The biological role of specific LOX isoforms has been recently clarified by an antisense approach and their depletion was able to influence plant development or pest/pathogen resistance [2,3].Transgenic potato plants depleted in the expression of a specific 9-LOX showed an abnormal tuber development [4].Furthermore Arabidopsis and potato transgenic plants with diminished levels of specific chloroplastic LOXs have reduced levels of wound inducible mRNAs [5,6]

LOXs are widespread in the seeds of many plant species;

in some cases such as soybean and other legumes they are abundant proteins and might also function as storage, rather than defence, proteins.This hypothesis is supported

Correspondence to A.Santino, ISPA-CNR, via Monteroni,

73100 Lecce, Italy.Fax:/Tel.: + 39 0832 420000,

E-mail: angelo.santino@irba.le.cnr.it

Abbreviations: 9-HODE,

(9S,10E,12Z)-9-hydroxy-10,12-octadeca-dienoic acid; 13-HODE,

(13S,9Z,11E)-13-hydroxy-9,11-octadeca-dienoic acid; LOX, lipoxygenase; RP-HPLC, reverse-phase HPLC;

SP-HPLC, straight-phase HPLC.

Enzyme: lipoxygenase (EC 1.13.11.12).

Note: a web site is available at http://www.ispa.cnr.it/

Note: The nucleotide sequence reported is in the EMBL database

under the accession number AJ417975.

*Present address: Institute of Sciences of Food Production C.N.R.

Bari, Italy.

(Received 18 July 2003, revised 2 September 2003,

accepted 12 September 2003)

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by the results on a soybean line lacking the three LOX

isoforms which shows similar crop performances in

com-parison to control lines [7].In other cases, LOX genes are

expressed only in early developmental stages when the

synthesis of storage proteins is not yet initiated.This has

been reported for maize L2 LOX [8], almond [9] and peanut

[10].It was reported that peanut LOX gene is also expressed

during Aspergillus colonization and consequently a possible

defensive role was suggested for this specific isoform [10]

However the physiological role of these LOXs is largely

unclear

Because of their role in the generation of pleasant or

unpleasant flavours and their involvement in co-oxidation

reactions leading to the bleaching of carotenoids and other

pigments, LOXs are also of great importance in food science

as they can influence the shelf life, the organoleptical and the

nutritional characteristics of seeds and other plant products

[11]

Hazelnuts are widely used in food industry with the

largest part of the world production adsorbed by the pastry

industry.Hazelnut seeds contain reasonable levels of linoleic

and linolenic acid (about 10 and 0.2%, respectively, of the

total fatty acids) and hexanal and nonanal are among the

most abundant volatile compounds detected in hazelnut oil

[12].Nevertheless LOX activity was not detected in mature

seed [13]

Considering the importance that LOXs could display in

influencing the shelf life and the organoleptic features of

hazelnut seeds, we carried out a study to characterize

hazelnut lipoxygenases at the biochemical and molecular

level

Materials and methods

Plant material

Hazelnut (Corylus avellana L.cv Mortarella) leaves and

seeds were harvested at different maturation stages from the

experimental field of the Istituto Sperimentale Frutticoltura,

Caserta.The leaves and shelled seeds were frozen in liquid

nitrogen and stored at)80 C

PCR amplification of hazelnut genomic probes

Two homologous probes (ln32, ln50) were obtained by

PCR using hazelnut genomic DNA as template, the

primers 5¢-CTATGATTATGATGTCTACAATGATTTG

GG-3¢ (ML1) and 5¢-GCAAATTCTTCATCAGTCATC

CATGCAGAC-3¢ (ML2) and the following amplification

conditions: 94C for 5 min (1 cycle); 94 C for 1 min,

45C for 1 min, 72 C for 2 min (25 cycles); 72 C for

5 min (1 cycle)

Construction and screening of the hazelnut

genomic library

Hazelnut (cv Mortarella) genomic DNA was extracted from

young leaves, and used for the construction of the library as

previously described [9]

The library was screened using ln32 and ln50

digoxigenin-labelled probes (Roche).The filters were washed at a final

stringency of 0.1· NaCl/Cit, 0.5% SDS, 65 C.Positive

plaques were picked and subjected to two additional screenings at the same conditions

RNA extraction and reverse transcription (RT) PCR analysis

Total RNA was isolated from 100 mg of hazelnut seeds using the Rneasy plant mini kit (Quiagen) following the manufacturer’s instructions.RT-PCR was per-formed using 2 lg of total RNA, oligo-(dT)18primer and the Superscript II Polymerase (Invitrogen) according to the manufacturer’s instructions.The first strand cDNA was used as template in PCR experiments with oligonucleotides designed on the basis of the genomic sequence

The 5¢ region of the hazelnut LOX cDNA was amplified using the following primers: 5¢-AAGATGAAACGTG AGACGG-3¢ (CA1); 5¢-GATGACATCTCCATGGAA TAC-3¢ (CA2).The 3¢ region of the hazelnut LOX cDNA was amplified using the following primers: 5¢-GTTT GGAAGAGAGATGCTGG-3¢ (CA3); 5¢-AAAGTTTTT AGATTGAGACACTATTGGGAATT-3¢ (CA4).PCR conditions were as follows: 94C for 3 min (1 cycle);

94C for 45 s, 50 C for 45 s, 72 C for 2 min (30 cycles);

72C for 15 min (1 cycle)

The amplified fragments were cloned in pCRII-TOPO vector (Invitrogen) and sequenced

For the semiquantitative RT-PCR, the cDNA was amplified with the following oligos: 5¢-GTATTCCATG GAGATGTCATC-3¢ (CA5); 5¢-AAAGTTTTTAGATTG AGACACTATTGGGAATT-3¢ (CA4).Actin cDNA was amplified using the following primers: 5¢-TGGTGTTAT GGTTGGTAT-3¢ (ACTFOR); 5¢-ACCTTCATCTTCAT GCTG-3¢ (ACTREV)

Densitometric analysis (using a Bio-Rad Gel Doc2000 and theQUANTITY ONE software) was carried out on the actin amplified fragments to normalize the amount of cDNA to be used in further PCR experiments

Protein extraction and lipoxygenase activity Lipid bodies were first isolated from soluble protein fraction as previously reported [9].LOX activity was assayed in total protein samples and in micro-somal fraction obtained by centrifugation of total pro-tein samples at 100 000 g for 30 min.The pellet (microsomal fraction) was resuspended in 100 mMsodium carbonate and the pH adjusted to 7.5 before assaying LOX activity

LOX activity was determined polarographically at 25C with a Clark O2electrode using linoleic acid as substrate Thirty micromolar stock solution was prepared according

to [14].The reaction mixture (1.0 mL) consisted 100 mM sodium phosphate buffer pH 6 containing 0.3 mMlinoleic acid and different amounts of protein samples.Decrease in

O2 concentration was monitored for 3 min and the enzy-matic activity was calculated from the initial rate of O2 uptake.One unit of LOX activity corresponds to the intake

of 1 lmol of O2per minute.pH optimum of hazelnut LOX was determined as previously described [9].LOX activity was also assayed spectrophotometrically monitoring the increase in A234 of the conjugated-diene structures as previously described [14]

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SDS/PAGE and Western blot analysis

Total proteins (20 lg) extracted from seeds harvested at

different developmental stages were subjected to SDS/

PAGE and transferred to nitrocellulose membrane

(Amer-sham).Western blot analysis was performed using the ECL

protocol (Amersham) and a 1 : 1000 dilution of the pea

LOX antibody [15]

Identification of lipoxygenase products

Protein samples from different developmental stages were

incubated for 1 h in 1 mL of 100 mMsodium phosphate

buffer pH 6 containing 0.3 mM linoleic acid.Reaction

products were reduced with sodium borohydride, extracted

with chloroform/methanol (2 : 1, v/v) and dried.The

reaction products were resuspended in methanol/water/

acetic acid (85 : 15 : 0.1, v/v/v) and separated by

reverse-phase HPLC (RP-HPLC) using a C18 Ultrasphere column

(Beckmann, 0.46· 25 cm) as already reported [9].The

absorbances at 234 and 210 nm were recorded

simulta-neously.The peak adsorbing at 234 nm containing the

hydroxy-10,12-octadecadienoic acid (HODE) isomers was

collected, dried and resuspended in n-hexane/propan-2-ol/

acetic acid (100 : 2 : 0.1, v/v/v) 9-HODE and 13-HODE

were separated by straight-phase HPLC (SP-HPLC) with

a Silica Ultrasphere column (Beckmann, 0.46· 25 cm) as

already described [9].The enantiomer composition of

9-HODE and 13-HODE was carried out by chiral

phase-HPLC on a Chiralcel OB column (Daicel Chem.Industries,

0.46· 25 cm, 5 lm particle size) with a solvent system of

hexane/propan-2-ol/acetic acid (100 : 5 : 0.1, v/v/v) and a

flow rate of 1 mLÆmin)1

Authentic standards of 9- and 13-HODE were purchased

from ICN.HPLC analyses were carried out using a

Beckman System Gold apparatus equipped with a 126

solvent module and a 168 detector

Extraction of genomic DNA and Southern blot analysis

Genomic DNA was extracted from young hazelnut leaves

using the Plant DNA isolation Kit (Roche).About 10 lg

genomic DNA were cleaved with EcoRI, BamHI and

HindIII, separated on a 0.8% agarose gel and transferred to

Hybond N membrane (Amersham).Hybridizations were

carried out at 65C overnight using homologous probes

digoxigenin labelled according to the manufacturer’s

instructions (Roche).Filters were washed at a final

stringency of 0.2· NaCl/Cit 65 C and chemiluminescent

detection was carried out using CDP-STAR as substrate

according to the manufacturer’s protocol (Roche)

Results

Lipoxygenase gene isolation and characterization

To identify and characterize hazelnut lipoxygenases at the

molecular level, we performed PCR experiments using

hazelnut genomic DNA as template and the primers ML1

and ML2 bordering a 937-bp conserved region (2103–3039)

of the soybean LOX3 gene [16].An amplification product

of about 700 bp was obtained in the above described

conditions.The amplified DNA was cloned and sequenced The results revealed that the amplification product con-tained two different lipoxygenase sequences showing a high degree of identity but belonging to different genes.The amplified sequences (ln32 and ln50) were used as homolog-ous probes to screen the hazelnut genomic library prepared

as described in methods.After three successive screenings

we isolated four different genomic clones using the ln32 and one clone with the ln50 probe

In order to identify a genomic clone containing a complete LOX gene, we hybridized the DNA extracted from all the clones with three probes corresponding to the 5¢, central and 3¢ portions of a previously isolated almond lipoxygenase gene [9].The results indicated that one of the clones identified (ln32/1) possibly contained a complete hazelnut lipoxygenase which was further characterized Figure 1 shows the 9887 bp characterized sequence and the hazelnut lipoxygenase gene organization.The sequence comprises 4180 bp 5¢-untranslated, an open reading frame

of 5334 bp encoding a putative protein with a molecular weight of 99 kDa and a 373-bp 3¢-untranslated region.The gene, named Lox1:Ca:1, contains nine exons and, as already observed for other lipoxygenase genes, a very large first intron of 1871 bp.Sequence analyses revealed that both the homologous probes, ln 32 and ln 50, comprise exon IV and ln 32 probe exactly matches the Lox1:Ca:1 gene from base 6790 to base 7444

FASTA analysis revealed that the hazelnut LOX gene shows the highest degree of identity with a almond LOX gene (79.5% [9]) High identity was also found towards a Gossypium hirsutum lipoxygenase induced by bacteria (75.5% [17]), an elicitor induced tobacco LOX (74.6% [18]); and some potato LOXs (74–72% [19–21])

The dendrogram reported in Fig.2 confirmed that the described hazelnut LOX is closely related to the almond, Gossypium, tobacco and potato LOXs

In the 5¢ upstream untranslated region, putative TATA and CAAT signals are present at position 4140 ()40 from the ATG) and 4066 ()114), respectively.In the 5¢ upstream untranslated region, we also found four inverted repeats (204–237 bp; 646–715; 1936–61; 2745–2923, bold in Fig.1); one of which is particularly large (177 bp)

LOX expression and enzymatic activity during hazelnut seed development

Hazelnut requires more than 6 months to complete seed development as, in Italy, it normally blossoms in December; seeds complete their development in the middle of July and are harvested at the end of August.The maturation stages considered in this work were identified on the basis of seed weight.Stage I (harvested at the end of May 2002) can be considered the beginning of cotyledon development.After this stage, the seeds were collected every 2 weeks until the middle of July (stages II, III and IV)

LOX expression was monitored by semiquantitative RT-PCR.Total RNAs extracted from different develop-mental stages were reverse transcribed using an oligo(dT) primer.The obtained cDNAs were used in PCR experi-ments with the LOX primers CA4 and CA5 (matching, respectively, from base 9488 to base 9520 and from base

8366 to base 8387 of the sequence reported in Fig.1) and

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Fig 1 Organization of the hazelnut lipoxygenase gene lox1:Ca:1 (A) Schematic representation of the hazelnut LOX gene indicating the translation start and the stop codon.The introns and exons are drawn in proportion to their length.(B) Nucleotide and deduced amino acidic sequences of the hazelnut LOX gene.The inverted repeats are in bold and their orientations are indicated by arrows.TATA and CAAT boxes and the initiating ATG are also in bold.

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Fig 1 (Continued).

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two primers designed on the basis of alignment results of

several plant actin genes

The LOX amplification product showed the expected size

(836 bp) and was further characterized by sequence

ana-lysis.The actin amplified fragment was also sequenced

As reported in Fig.3, hazelnut LOX is mainly expressed

during early maturation stages (stages I and II).A faint

band is visible in the other maturation stages in overloaded

gels.The same RT-PCR experiments, conducted on RNA

samples from young leaves, did not reveal any expression of

this gene in this organ (data not shown)

To verify the expression of the LOX gene corresponding

to the ln50 clone, two specific oligos were designed and used

in RT-PCR experiments.In our experimental conditions we

were not able to observe any expression of this gene in seed

or in leaves (not shown)

We carried out Western blot analysis on total protein

samples from hazelnut seeds at different developmental

stages using pea LOX antibodies [15].As reported in Fig.3,

a polypeptide in the molecular mass range expected for

LOXs (99 kDa) was detected in protein samples from stage I

and II seeds

To analyze LOX activity throughout seed development

we set up a procedure aimed to reduce the interference of

endogenous lipids on enzymatic assay.For this reason the

lipid bodies fraction was first removed and LOX activity

was assayed in total protein samples or in the microsomal

fraction

The enzymatic activity was preliminarily analyzed at

different pH values (pH 5–9) and we found that the

hazelnut LOX has a pH optimum of about 6.In these experimental conditions, LOX activity was detected in all the developmental stages considered with a maximum in

Fig 2 Phylogenetic tree of hazelnut LOXs The amino acid sequences of hazelnut lipoxy-genases were compared with other plant LOXs (accession numbers are in parentheses) The phylogenetic tree was obtained using the PHYLIP (Phylogeny Inference Package) program.

Fig 3 Analysis of LOX activity and LOX gene expression in hazelnut seedat d ifferent d evelopmental stages Hazelnut seeds, collected at different maturation stages, were weighed (A) and used to extract total proteins for LOX immunodetection and LOX activity quantification Twenty micrograms of total proteins were separated by SDS/PAGE, transferred to nitrocellulose and LOX was immunodetected with a pea LOX antibody (B).LOX activity was assayed measuring the con-sumption of oxygen (nmolÆmin)1Æmg)1protein) with a Clark electrode using linoleic acid as a substrate (C).cDNAs were generated using an oligo(dT) 18 primer and total RNA extracted from the different mat-uration stages.PCR experiments were carried out with LOX specific primers (D) or with actin specific primers as internal control (E).

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stage I.After this stage it declined throughout seed

development and was negligible in mature seed (Fig.3)

We also tested the presence of LOX activity in either the

microsomal or the lipid bodies fractions (data not shown)

In both these fractions, low levels of LOX activity were

recorded but at present it is unclear if the same LOX

isoforms found in the soluble fraction are responsible for

this activity or if it derives from other isoforms

Plant LOXs are usually classified as 9-LOXs and

13-LOXs on the basis of their product specificity.In order

to better characterize the hazelnut LOX we analyzed by

RP-HPLC the reaction products using linoleic acid as substrate

The reaction products were reduced with sodium

boro-hydride and separated by RP-HPLC.The peak adsorbing

at 234 nm containing the hydroperoxides was collected and

subjected to SP-HPLC to separate 13- and 9-HODE.The

retention times of the reaction products of the hazelnut

LOX were compared with the reaction products of soybean

LOX type I and authentic standards of 9- and 13-HODE

As shown in Fig.4, 9-HODE is the main product of the

hazelnut LOX reaction (about 70% of total

hydroper-oxides).We carried out chiral-phase HPLC on both 9- and

13-HODE to separate R and S enantiomers.As reported in

Fig.4 the products of hazelnut LOX are predominantly in

the S configuration indicating that these compounds derive

from the activity of a specific lipoxygenase

Similar results were obtained using linolenic acid as

substrate (data not shown).From these results we can

conclude that a 9-LOX is largely responsible for the LOX activity in immature hazelnut seed

In order to correlate LOX activity and the production of

C6 and C9 aldehydes deriving from the activity of other enzymes of the LOX pathway, we carried out a gas-chromatographic analysis of the head space volatiles compounds present in the hazelnut seeds at different developmental stages.Both C6and C9aldehydes (and the corresponding alcohol) were detected in all the samples and, similarly to the pattern of LOX expression and activity, their levels were higher in stage I seed and rapidly decline during maturation (data not shown)

LOX cDNA isolation and characterization

To better characterize LOX mRNAs expressed in hazelnut seeds, we performed RT-PCR experiments using RNA extracted from hazelnut immature seeds.Primers were synthesized on the basis of the sequence of the isolated genomic clone.Attempts to amplify a complete LOX cDNA in a one-step PCR amplification were unsuccessful,

so we used two pairs of oligonucleotides to obtain separately the 5¢ and 3¢ regions.The amplified fragments were cloned and sequenced.The 5¢ (1757 nt) and the 3¢ region (1487 nt) overlapped for 672 nt and were considered different portions of the same gene.The 2572 bp cDNA (CaLOX1) corresponded exactly to the deduced cDNA from the genomic clone Lox1:Ca1, but missed the first 51 bp at the 5¢ end as the sense primer was designed considering the ATG located at position 4235 of the genomic clone as the translation start.The characterization of other clones revealed the presence of another cDNA (CaLOX2) sharing high identity, 91.9%, with the CaLOX1.The comparison

of the deduced amino acidic sequences of CaLOX1 and CaLOX2 indicated that the two proteins differ in 68 positions

Considering the high degree of identity of the two cDNAs, the expression results obtained by semiquantitative RT-PCR reported in Fig.3 have to be considered as the sum of the expression of both CaLOX1 and CaLOX2.The sequence of 10 independent clones deriving from RT-PCR experiments, however, revealed that nine corresponded to CaLOX2 and one to CaLOX1, suggesting that CaLOX2

is the predominant LOX cDNA in hazelnut seeds After comparison with other plant LOXs (almond, cotton, Arabidopsis, tomato, potato and soybean LOX1)

we verified the presence of all of the most conserved regions (Fig.5).Among these are the conserved domains involved

in substrate binding (AWRTDEEFGREMLAG, positions 373–387) and in oxygen binding (ASALHAAVNFGQY, positions 723–735).The highly conserved C-terminal motif GIPNSVSI is also present.The histidine residues (His535, His540, His727), asparagine (Asn731) and isoleucine (Ile873) essential for active site iron binding are present at the expected positions.The TV motif, thought to be characteristic of 9-LOXs [22], is present in both the two identified cDNAs (at positions 591–592 of Lox1:Ca:1) Southern analysis

Southern blot analysis of hazelnut DNA was carried out by probing two different regions spanning the 5¢- (1757 bp)

Fig 4 HPLC analysis of hydroxyl-fatty acids produced by the hazelnut

LOX Two hundred micrograms of total proteins from immature

hazelnut seed were incubated for 30 min in 0 1 M sodium phosphate

buffer pH 6 containing 0.3 m M linoleic acid.Reaction products were

first separated by RP-HPLC and then by SP-HPLC as described in

Materials and methods.Inset shows the retention time of the isomers

produced by soybean LOX1 compared with authentic standards of

9- and 13-hydroxy linoleic acid.Boxes: chiral phase HPLC showing the

positional isomers composition of 13- and 9-HPOD.

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and 3¢-end (836 bp) of the isolated CaLOX2 A simple

hybridization pattern was obtained with both the probes

Figure 6 shows the hybridization signals obtained with the

836 bp fragment corresponding to the 3¢ portion of the

cDNA.On the basis of restriction analysis of the genomic clone, a 1897-bp fragment was expected in the EcoRI digestion; a fragment larger than 1627 bp fragment was expected with the HindIII digestion and a fragment larger

Fig 5 Comparison of the cDNA-deduced protein sequences of hazelnut LOXs Sequences were aligned using the CLUSTALW 1.7 program Hazelnut CaLOX1 refers to the putative protein from the genomic clone Lox1:Ca:1 (accession no.AJ417975), hazelnut CaLOX2 is deduced from the cDNA clone (CaLOX2) described in the text.The other aligned plant LOXs were as follows: almond (accession no.AJ404331), cotton (accession number AF361893), Arabidopsis lox1 (accession no.JQ2267), tomato loxA (accession number P38415), tomato loxB (accession number P38416), potato lox1 (accession no.U60200) and soybean lox1 (accession no.J02795).

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than 3387 bp was expected with the BamHI digestion.The

most intense signals visible in Fig.6 correspond to these

fragments, while the faint hybridization signals could

indicate the presence of other LOX genes

Discussion

PCR experiments carried out on genomic DNA resulted in

the amplification of two different LOX sequences (ln32 and

ln50).A genomic clone was shown to contain a complete

LOX gene (Lox1:Ca:1) RT-PCR experiments, performed

with RNA from immature seeds, revealed the presence of

two different LOX cDNAs, one of which corresponded

exactly to the characterized Lox1:Ca:1 gene.The second

clone shared a high degree of similarity (91.9% identity at

the amino acid level) and is encoded by a different LOX

gene.Sequence results and Southern blot analysis

collec-tively identified the presence of three different types of LOX

gene in the hazelnut genome; it is likely that more will be

detected with time.Most plant species have multiple LOX

genes in several classes, including tomato, potato, pea,

soybean and Arabidopsis [23,24]

Although the numbers and relative positions of introns

within plant LOX genes are fairly constant, their length

varies and this is particularly marked in relation to intron I, which can vary in length from 111 to 1245 bp in Arabidopsis LOXgenes, be as large as 1201 bp in almond seed LOX [9]

or even 2542 bp in the Glycine max L-4 gene (see [25]).The lox1:Ca:1first intron is 1871 bp

There is some evidence to suggest that those LOX genes expressed predominantly in vegetative tissues have parti-cularly large first introns (see [25] for references).In this regard, the lox1:Ca:1 gene is interesting because it is expressed only at early stages of embryo development and not during the mid-to-late maturation phases of seed development, in a fashion reminiscent of the pea C2 LOX, the RNA for which is detected only at very early stages of seed development, and which is the only LOX detected in pea leaves [25].Considering the high level of expression of CaLOX2in hazelnut seeds, it would be of interest to isolate and characterize the corresponding genomic clone in order

to determine if it has a similar genomic organization to Lox1:Ca:1

Hazelnut CaLOX1 and CaLOX2 seem not to be expressed in leaves.At present the physiological role of hazelnut seed LOXs is unclear LOX gene expression, the enzymatic activity, and the accumulation of LOX protein in developing seeds could be associated with the intense mitotic activity and the consequent rapid remodelling of cell membranes occurring in developing seed.FASTA analysis suggests that, despite the clear evidence for expression in early seed development, the lox1:Ca:1 gene

is more similar to some vegetatively/tuber-expressed LOX genes than those expressed in seeds.Possibly the conditions

in the very early stages of seed development, when growth is mitotic rather than through differentiation and cell expan-sion, promote the expression of Lox1:Ca:1.The 5¢-non-coding promoter sequence of lox1:Ca:1 contains a number

of putative transcription factor binding motifs, and also inverted repeats that could form stem loop structures reminiscent of those proposed for the promoter of the pea lox1:Ps:3gene [26].The functional significance of any such elements is unknown and requires further analysis The hazelnut lipoxygenase shows dual product specificity, forming a mixture of 9- and 13-hydroperoxides in an approximate 2 : 1 ratio.This is not uncommon; pea seed LOX-3, for instance, also produces 9- and 13-hydroper-oxides from linoleic acid in a 2 : 1 ratio.Pea seed LOX-3 additionally produces keto-fatty acids, which are thought to arise from the dismutation of a prematurely released fatty acid peroxyl radical [27].The hazelnut lipoxygenase does not, however, form such products, indicating that there is no particular link between dual product specificity and keto-fatty acid production (see also [23])

There are a number of similarities between the hazelnut and almond seed lipoxygenases [9].Their amino acid sequences are 80% identical; they have a similar pH optimum; and they both produce 9-hydroperoxides from linoleic acid, although the LOX activity (in terms of specific activity) is much higher in almond.The almond LOX, however, produces exclusively 9-hydroperoxides, whereas the hazelnut LOX forms a mixture of 9- and 13-products LOXgene expression, enzymatic activity and the synthesis

of C6and C9aldehydes all have a similar trend throughout hazelnut seed development, being fairly limited to the early developmental stages.It is likely that the synthesis of these

Fig 6 Southern hybridization of hazelnut genomic DNA with a

digo-xigenin-labelled LOX probe Genomic DNA (10 lg) was digested with

HindIII (H); BamHI (B) and EcoRI (E) and hybridized with an 836-bp

fragment from the 3-end of the hazelnut CaLOX2.DNA size

stand-ards in kb are shown to the left.

Trang 10

molecules is a consequence of the LOX and hydroperoxide

lyase activities.Further studies are in progress to clarify the

role of these enzymes in the production of volatile

compounds, which are important constituents of hazelnut

flavour and aroma

The hazelnut and almond LOXs are closely related to

some plant LOXs involved in plant response to biotic

stresses.Among these, the highest identity was found

towards a cotton LOX, induced in the hypersensitive

reaction towards Xanthomonas campestris.Jalloud and

coworkers [17] showed that this cotton LOX is a 9-LOX

and (9S)-hydroperoxides are largely predominant during

the hypersensitive response of cotton cells.A high degree

of identity (74.6%) was also found towards the tobacco

9-LOX specifically induced by Phytophthora parasitica [18]

The importance of this 9-LOX in the resistance to this

pathogen was further confirmed in transgenic tobacco

plants, in which the activity of this specific LOX was

down-regulated by an antisense strategy.In contrast to

wild type plants, transgenic plants became susceptible to

Phytophthora parasitica[28]

Despite these clear indications on the importance of

9-LOXs in plant defence, the nature and the biological

activities of oxylipins produced from 9-hydroperoxides are

still largely unclear.Recently Go¨bel et al.[29] reported that

cultured potato cells treated with a Phytophthora infestans

elicitor accumulated high levels of 9-LOX and 13-LOX

However, oxylipin profiling revealed that the main oxylipins

detected in treated potato cells were derived from the

9-hydroperoxides.Among these are colneleic and colnelenic

acids which are produced by the activity of the divinyl ether

synthase [30,31] and may act as antifungal molecules

inhibiting the germination of the fungal spores [32]

Moreover some other oxylipins deriving from

9-hydro-peroxides such as 10-oxo-11,15-phytodienoic acid

(10-OPDA), have been shown to display a regulatory

function in response to biotic stresses as well as in plant

developmental processes [33].This could suggest an

import-ant role for 9-LOX metabolism.The importance of

oxylipins derived from 9-LOX metabolism in seed

develop-ment has not yet been demonstrated.Further investigation,

aiming to evaluate the expression of other genes of the

lipoxygenase pathway involved in oxylipin biosynthesis

(allene oxide synthase, hydroperoxide lyase), will help to

elucidate the role of the LOX pathway in developing seeds

Acknowledgements

We are grateful to Dr Claire Domoney for the gift of pea LOX

antibodies, Dr Pasquale Piccirillo for the hazelnut agronomic aspects,

Dr Danilo Dello Monaco for GC-MS analysis, Professor Liugino

Troisi for chiral phase HPLC analyses and Mr Leone D’Amico for

technical assistance.

This work was supported by Ministero dell’Universita` e della

Ricerca Scientifica e Tecnologica, Cluster C03.

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