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Tiêu đề Fatty acid desaturases from the microalga Thalassiosira pseudonana
Tác giả Thierry Tonon, Olga Sayanova, Louise V. Michaelson, Renwei Qing, David Harvey, Tony R. Larson, Yi Li, Johnathan A. Napier, Ian A. Graham
Trường học University of York
Chuyên ngành Molecular biology
Thể loại Research article
Năm xuất bản 2005
Thành phố York
Định dạng
Số trang 12
Dung lượng 266,68 KB

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Nội dung

For biotechno-logical applications, these organisms are regarded as Keywords desaturases; long chain polyunsaturated fatty acids; sphingolipids; Thalassiosira pseudonana; yeast expressio

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Thierry Tonon1,*, Olga Sayanova2, Louise V Michaelson2, Renwei Qing1,†, David Harvey1,

Tony R Larson1, Yi Li1, Johnathan A Napier2and Ian A Graham1

1 CNAP, Department of Biology, University of York, Heslington, York, UK

2 Rothamsted Research Institute, Harpenden, UK

The algae, as a group, represent the third largest

aqua-culture crop (after freshwater fish and molluscs) in the

world today [1,2] In recent years, considerable

atten-tion has been directed at marine microalgae for the

production of oils and fatty acids, in particular the use

of algal oils containing long chain polyunsaturated

fatty acids (LCPUFAs) The most prominent of these

are the health beneficial omega-3 eicosapentaenoic acid (EPA, 20:5D5,8,11,14,17) and docosahexaenoic acid (DHA, 22:6D4,7,10,13,16,19) Among the alga groups iden-tified as producers of high levels of LCPUFAs, di-atoms are able to produce and accumulate EPA and DHA in triacylglycerols (TAGs) [3] For biotechno-logical applications, these organisms are regarded as

Keywords

desaturases; long chain polyunsaturated

fatty acids; sphingolipids; Thalassiosira

pseudonana; yeast expression

Correspondence

I A Graham, Department of Biology

(area 7), University of York, PO Box373, UK

Fax: +44 1904 328762

Tel: +44 1904 328750

E-mail: iag1@york.ac.uk

Present addresses

*UMR 7139, CNRS-GOEMAR-UPMC,

Station Biologique, BP 74, 29682 Roscoff

cedex, France

 College of Life Science, Sichuan University,

Chengdu, China

Note

The sequences reported in this paper have

been submitted to GenBank database under

the accession number AY817152 (TpdesO),

AY817153 (TpdesA), AY817154 (TpdesB),

AY817155 (TpdesI) and AY817156 (TpdesK)

(Received 13 March 2005, revised 22 April

2005, accepted 9 May 2005)

doi:10.1111/j.1742-4658.2005.04755.x

Analysis of a draft nuclear genome sequence of the diatom Thalassiosira pseudonana revealed the presence of 11 open reading frames showing significant similarity to functionally characterized fatty acid front-end desaturases The corresponding genes occupy discrete chromosomal loca-tions as determined by comparison with the recently published genome sequence Phylogenetic analysis showed that two of the T pseudonana desaturase (Tpdes) sequences grouped with proteobacterial desaturases that lack a fused cytochrome b5 domain Among the nine remaining gene sequences, temporal expression analysis revealed that seven were expressed

in T pseudonana cells One of these, TpdesN, was previously characterized

as encoding aD11-desaturase active on palmitic acid From the six remain-ing putative desaturase genes, we report here that three, TpdesI, TpdesO and TpdesK, respectively encode D6-, D5- and D4-desaturases involved

in production of the health beneficial polyunsaturated fatty acid DHA (docosahexaenoic acid) Furthermore, we show that one of the remaining genes, TpdesB, encodes aD8-sphingolipid desaturase with strong preference for dihydroxylated substrates

Abbreviations

ARA, arachidonic acid; DHA, docosahexaenoic acid; EPA, eicosapentaenoic acid; EST, expressed sequence tag; FAME, fatty acid methyl ester; gDNA, genomic DNA; LCB, long chain base; LCPUFA, long chain polyunsaturated fatty acid; PUFAs, polyunsaturated fatty acids; RACE, rapid amplification of cDNA ends; TAG, triacyglycerol; Tpdes, Thalassiosira pseudonana desaturase.

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potentially good sources for the cloning of genes

enco-ding the enzymes required for LCPUFA biosynthesis

Different routes of LCPUFA synthesis have developed

in nature The production of EPA and DHA in marine

bacteria and some marine fungi relies on anaerobic

polyketide synthase systems, which are encoded by

sev-eral large polypeptides [4] More gensev-erally,

biosynthe-sis of these fatty acids requires aerobic desaturases and

elongases that catalyse a consecutive series of

desatura-tion and elongadesatura-tions of the fatty acyl chain to generate

EPA and DHA from a-linolenic acid (18:3D9,12,15)

Besides the main routes leading to DHA viaD6

-desatu-ration, some algae display an alternate pathway for

C20-PUFA production involving aD9-elongase [5] and

aD8-desaturase [6]

To date, at least one enzyme corresponding to each

of the front-end desaturases and elongases necessary

to convert a-linolenic acid to EPA has been isolated

from diverse origins [7] ‘Front-end’ desaturation can

be defined as desaturation between a pre-existing

dou-ble bond and the C-terminal end of a fatty acid, as

opposed to the much more prevalent (in plants)

methyl-directed desaturation Reconstitution of EPA

biosynthesis has been achieved in yeast [8,9] and in

plants [10,11], with encouraging levels of

C20-LCPUFA production Moreover, the D4-desaturase

gene encoding the last step in DHA biosynthesis has

recently been isolated from a number of marine

organ-isms [12–14] The final elongation step [of C20

polyun-saturated fatty acids (PUFAs) to C22] catalysed by a

D5-elongase was the last outstanding step remaining to

be functionally characterized at the molecular level

Very recently, characterization of such an activity has

been described in the microalgae Pavlova lutheri [15],

Ostreococcus tauri and Thalassiosira pseudonana [16]

These novel fatty acid elongases were used to

success-fully reconstitute DHA synthesis in yeast Therefore,

all the activities are now available to engineer plants to

produce this nutritionally important fatty acid

How-ever, all these enzymes have been isolated from a

diverse array of organisms, for instance several marine

microalgal species For the purposes of metabolic

engineering and in order to achieve optimal synthesis

in a heterologous host, it may be advantageous to use

a complementary set of desaturase and elongase

enzymes from the same organism This may be

partic-ularly relevant for the metabolic engineering of a

com-pound such as DHA in a heterologous host such as

linseed which would require the introduction of three

desaturase and two elongase steps in order to convert

the endogenous fatty acid a-linolenic acid to DHA

Gene discovery-based strategies such as targeted

expressed sequence tag (EST) databases or PCR

amplification using degenerate primers typically do not provide sufficient coverage to enable identification of complete sets of genes for a particular process from a single organism Bioinformatics-based analysis of com-plete genome sequences potentially allow an exhaustive approach to gene discovery from a single organism if the process in question is sufficiently understood in terms of enzymes and other proteins involved at the biochemical level Such a situation now exists for dis-covery of genes involved in PUFA biosynthesis follow-ing the completion of the genome sequence of the EPA and DHA producing diatom T pseudonana [17] Levels

of EPA and DHA in this organism are in the range of

17 and 5%, respectively, when in the exponential phase

of growth [3] Two elongases involved in LCPUFA biosynthesis from T pseudonana have been recently characterized [16] and analysis of a draft genome sequence of this organism prior to publication of the complete genome sequence revealed the presence of a family of putative front-end desaturases that are obvi-ous candidates for enzymes involved in the synthesis of EPA and DHA [18] However, rather surprisingly, the first of these genes to be functionally characterized was found to encode a cytochrome b5 fusion desaturase exhibiting D11-desaturase activity Here we report the cloning and characterization of the three desaturases involved in DHA synthesis, i.e a D6-, a D5- and a

D4-desaturase Moreover, heterologous expression of

an additional cytochrome b5 fusion desaturase has allowed the identification of a new D8-sphingolipid desaturase from Thalassiosira

Results

Phylogenetic and expression analysis of

T pseudonana genes with similarity to front-end desaturases

A recent phylogenetic analysis of the draft genome sequence of T pseudonana [18] reported the presence

of 12 sequences showing significant similarity to func-tionally characterized front-end desaturases, i.e a fused cytochrome b5 binding domain at their N-termi-nus and three histidine boxes [19] Now that contigs have been built for the entire genome and most assigned to 24 nuclear chromosomes [17], we re-exam-ined these 12 putative desaturase sequences based on cDNA characterization and genome analysis In our previous analyses, two partial desaturase coding sequences present near the ends of two distinct contigs were designated as unique genes, TpdesB and TpdesD TpdesB encoded an N-terminus region and TpdesD encoded a C-terminus region Our subsequent cDNA

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analysis of these sequences has revealed that they

actu-ally represent a single gene present on chromosome 4

that is from now on referred to as TpdesB

Compar-ison of the full-length TpdesB cDNA with the genomic

sequence demonstrated that no introns are present in

the gene The TpdesB ORF gives a predicted protein

of 493 amino acids A further annotation update

relates to TpdesH which, based on EST sequence

ana-lysis, appears to contain three characteristic histidine

boxes but lacks the N-terminal cytochrome b5 domain

TpdesL is a close homolog of TpdesH that also lacks

the cytochrome b5 domain Both these genes share

higher overall sequence similarity with putative

proteo-bacterial desaturases that typically contain three

histi-dine boxes but also lack the cytochrome b5 fusion

domain; for this reason they were excluded from the functional analysis described in this present study Based on information contained in the GenBank data-base we have allocated 10 of the 11 T pseudonana Tpdes sequences to specific chromosomes (Fig 1A) These 10 Tpdes sequences are distributed among six of the 24 chromosomes, with three sequences on chromo-some 5, two on chromochromo-somes 4 and 6, and one each on chromosomes 3, 7 and 21 Material used to sequence the T pseudonana genome was derived from a single diploid founder and this revealed the presence of two haplotypes with on average 0.75% polymorphism at the nucleotide level [17] However, the Tpdes genes occupy distinct chromosomal positions and therefore even the pairings with highest sequence similarity such

Fig 1 Evolutionary relationship of T pseudonana putative desaturases (TpDES) with known front end desaturases and expression analysis

of corresponding genes T pseudonana sequences were arbitrarily designated TpDESA to TpDESO (A) The phylogenetic tree of TpDES and functionally characterized front-end desaturases was established using the PHYLIP 3.5c software package and based on 148 alignable amino acid residues [18] Percentage bootstrap values above 60 are indicated above the nodes Chromosome location and availability of cDNAs for each gene is shown after the gene name (B) For RT-PCR based gene expression analysis, cells were harvested at various time of incubation and growth stage monitored by measuring the percentage of nitrogen degraded (inset table) PCR analysis was performed with gene speci-fic primers on undiluted (lane 1) and five-fold serial dilutions (lanes 2–4) of cDNA Size of the expected cDNA amplified fragment is indicated

in brackets below the gene name Inset PCR products from genomic DNA are shown in order to validate the TpdesG and TpdesM primer pairs M, DNA molecular size ladder.

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as TpdesO-TpdesM, TpdesN-TpdesG and

TpdesH-TpdesLare not due to haplotype variation

The phylogenetic tree of TpDES sequences was

re-constructed with the updated Tpdes sequences noted

above in combination with front-end desaturases from

a range of organisms The resulting tree shows three

major groupings containing TpDES sequences

(Fig 1A) The first group, containing TpDESL,

TpDESH and four proteobacterial sequences, is

char-acterized by the lack of a fused cytochrome b5

domain None of these genes have been functionally

characterized and we did not include TpDESL or

TpDESH in our functional analysis The remaining

nine Tpdes genes show significant similarity to other

functionally characterized desaturases As a first step

to characterizing the Tpdes genes we analysed temporal

expression analysis throughout the growth phases of

the algal cell culture using semiquantitative RT-PCR

(Fig 1B) The second phylogenetic group contains

TpDESN together with previously characterized

D5- andD4-desaturases TpDESO and TpDESM group

with the diatom Phaeodactylum tricornutum D5

-desatu-rase PtDEL5 (Fig 1A) Comparison of genomic

sequences of TpDESO and TpDESM showed 72%

identity, and one intron could be detected in each

sequence RT-PCR analysis revealed that of these two

genes only TpdesO is transcribed (Fig 1B) The

TpdesOORF is 1425 bp long and encodes a protein of

474 amino acids Alignment with the corresponding

genomic sequence confirmed the presence of a 99 bp

intron in the TpdesO gene The amino acid sequence

of PtDEL5 and TpDESO exhibited 63% identity,

sug-gesting that TpDESO could catalyse the D5

-desatura-tion step in the PUFA biosynthetic pathway The

TpDESK gene sequence forms a subgroup with

func-tionally characterized D4-desaturases from

Thrausto-chytrium sp and Euglena gracilis (Fig 1A) TpDESK

is expressed at a low level relative to TpdesO during

the exponential phase of growth TpDESN and

TpDESG do not group with functionally characterized

front-end desaturases from other organisms TpDESN

has already been characterized as a 16:0 specific

D11-desaturase [18] Alignment of the TpdesG genomic

sequence with other desaturases showed that although

it contains a cytochrome b5 domain and three histidine

boxes a start methionine cannot be determined by

in silicoanalyses alone, indicating that it may represent

a pseudogene RT-PCR based expression analysis

sug-gested that the gene is not expressed during the growth

phase and we have not investigated it further In the

third major group, TpDESE, TpDESI, TpDESB and

TpDESA are separated on four branches (Fig 1A)

The TpdesE ORF is incomplete in the draft genome sequence in comparison to other desaturases, and 5¢-RACE experiments failed to produce full-length cDNA for this gene despite the fact that it shows relat-ively high mRNA expression levels throughout the growth phases TpdesI is similarly highly expressed and the corresponding full length amino acid sequence has 70% sequence identity and groups with the Phaeod-actylum tricornutum PtDEL6 D6-desaturase TpdesI contains an intron of 149 bp, and the corresponding cDNA contains a 1455 bp ORF giving a predicted polypeptide of 484 amino acids The remaining two TpDES sequences, TpDESB and TpDESA, showed only 25% identity at the amino acid level Comparison

of TpdesA genomic and cDNA sequences revealed that the gene contains three introns of 84, 88 and 68 nucle-otides The 1548 bp cDNA of TpdesA gives a predicted polypeptide of 515 amino acids No function could be predicted for these enzymes from comparison of their primary structure with other front-end desaturases as they do not cluster with any functionally characterized desaturases with significant confidence

Incorporation of intron presence and positional information in genomic sequences does not shed any further light on the phylogenetic relationship of the cytochrome b5 containing T pseudonana desaturase genes TpdesB and TpdesN do not contain introns, TpdesK, TpdesO and TpdesI each have a single intron and TpdesA contains three introns Full-length cDNAs are not available for TpdesG and TpdesE therefore definite information on intron position is not available for these two genes Intron⁄ exon junction is not con-served between any pair of the Tpdes genes analyzed and our analysis suggests that introns appear to have evolved independently in each case

Characterization of PUFAs front-end desaturases

To establish the function of the different putative front-end desaturases, the full-length cDNAs of TpdesA, TpdesB, TpdesI, TpdesK and TpdesO were cloned into the vector pYES2, under the control of an inducible galactose promoter, to produce the constructs pYDESA, pYDESB, pYDESI, pYDESK and

pYDES-O They were first expressed in the Saccharomyces cere-visiae strain Invsc1 (or W303A1 for pYDESK) Transformants were incubated in the presence of a range of potential fatty acid substrates (18:2D9,12, 18:3D9,12,15, 20:2D11,14, 20:3D11,14,17, 20:3D8,11,14, 20:4D8,11,14,17, 22:4D7,10,13,16, 22:5D7,10,13,16,19) of desatu-rases involved in the PUFA biosynthesis pathway After addition of such substrates, no new peaks were detected for pYDESA and pYDESB, indicating that

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these desaturases were not involved in production of

LCPUFAs However, comparison of fatty acid profiles

derived from yeast transformed with pYES2 and

pYDESI showed two new peaks in the TpdesI

trans-formants even in the absence of exogenous fatty acids

in the medium These new peaks corresponded to

16:2D6,9and 18:2D6,9(Fig 2) These fatty acids are

pro-duced byD6-desaturation of 16:1D9and 18:1D9,

respect-ively, the two major fatty acids found in yeast When

linoleic (18:2D9,12) and a-linolenic (18:3D9,12,15) acids

were added to the culture medium, 18:3D6,9,12 and

18:4D6,9,12,15 were detected (Fig 2), confirming that

TpdesI encodes a D6-desaturase Analysis of the fatty

acid composition in the pYDESI transformants after

6 days of incubation showed the percentage conversion

of the 16:1D9 and 18:1D9 substrates were 29 and 38%,

respectively For the exogenous substrates 18:2D9,12 and 18:3D9,12,15, TpDESI exhibited a slight preference for the omega-3 fatty acid, as 68 and 80% of these substrates were converted to their corresponding

D6-products

Fatty acid profiling of extracts from TpDESO

S cerevisiae transformants detected new peaks when the culture medium was supplemented with 20:3D8,11,14 and 20:4D8,11,14,17 (Fig 3A) These new FAMEs were identified as 20:4D5,8,11,14 (arachidonic acid, ARA) and 20:5D5,8,11,14,17 (EPA), respectively These results dem-onstrate that pYDESO introduces a double bond at position 5 from the C-terminus of 20:3D8,11,14 and 20:4D8,11,14,17, indicating it is a D5-desaturase Analysis

of cells harvested after incubation for 6 days in the presence of both fatty acid substrates showed 16–19% conversion of each to their corresponding D5 fatty acids, suggesting that pYDESO does not have a

Fig 2 GC analysis of FAMEs from yeast transformed with the

empty plasmid pYES2 or the plasmid containing TpDESI Yeast

cells transformed with either pYES2 (bottom chromatogram) or

pYDESI (top chromatogram) were induced for six days in the

pres-ence of 18:2D9,12and 18:3D9,12,15exogenously fed before sampling

for fatty acid analysis New fatty acids are underlined I.S., internal

standard (17:0) The experiment was repeated twice and results of

a representative experiment are shown.

Fig 3 GC analysis of FAMEs from yeast transformed with the empty plasmid pYES2 or the plasmid containing TpDESO Yeast cells transformed with either pYDESO (top chromatograms) or pYES2 (bottom chromatograms) were induced for six days in the presence of 20:3 D8,11,14 and 20:4 D8,11,14,17 (A), 20:3 D11,14,17 (B), and 20:2 D11,14 (C) exogenously fed before sampling for fatty acid analy-sis New fatty acids are underlined The experiment was repeated twice and results of a representative experiment are shown.

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preference for one substrate over the other The

Cae-norabditis elegans D5-desaturase is capable of inserting

double bonds in a nonmethylene interrupted pattern

into 20:2D11,14 and 20:3D11,14,17 as well as in a

methy-lene interrupted pattern into fatty acids with aD8

dou-ble bond [20] TpdesO transformants were incubated in

the presence of 20:3D11,14,17 and 20:2D11,14 to establish

if the T pseudonana enzyme exhibited similar

charac-teristics Profiling of extracts of TpdesO transformants

fed with 20:3D11,14,17 and 20:2D11,14 revealed the

pres-ence of new peaks in both corresponding to

20:4D5,11,14,17 (juniperonic acid) and 20:3D5,11,14

(podo-carpic acid), respectively (Fig 3B,C) The percentage

conversion of 20:2D11,14and 20:3D11,14,17to theirD5

-de-saturated products was 4.7 and 8.4, respectively, which

was significantly less than the percentage conversion

determined for D5-desaturation of the D8-desaturated

fatty acids 20:3D8,11,14and 20:4D8,11,14,17

Heterologous expression of TpDESK in S cerevisiae

identified this enzyme as a D4-desaturase, as feeding of

transformants with 22:5D7,10,13,16,19 resulted in the

appearance a new peak identified as 22:6D4,7,10,13,16,19

(Fig 4) The quantities of both D4-desaturated FAs

detected were low but significant, with a conversion value of 3.0% for DHA These were the only unique peaks detected in the TpDESK transformants fed with the full range of fatty acids compared to the empty vector pYES2 controls

Characterization of sphingolipid related front-end desaturase(s)

Previous data have demonstrated that sphingolipid long chain base (LCB) desaturases have a paralogous relationship to front-end PUFA desaturases To deter-mine if any of the five T pseudonana cytochrome b5 fusion candidate desaturases (TpdesA, TpdesB, TpdesI, TpdesK and TpdesO) functioned as sphingolipid desaturases, LCBs were extracted from S cerevisiae cells after galactose-induced expression of the heterolo-gous gene Total LCBs (i.e both free LCBs and those deacylated from sphingolipids) were extracted and ana-lysed using previously reported methodology [21] LCB desaturation was determined by separation of deri-vatized LCBs by HPLC and LC-MS as previously described [22], with candidate T pseudonana enzymes tested for activity using both trihydroxy (i.e phyto-sphingosine) and dihydroxy (i.e sphinganine) sub-strates Of the five candidate desaturases tested by expression in S cerevisiae, only one, TpdesB, displayed any ability to desaturate sphingolipid LCBs, resulting

in the appearance of one additional (non-native) LCB (Fig 5) This activity was more pronounced when the pYDESB plasmid was expressed in the yeast sur2D mutant (which lacks the LCB C-4 hydroxylase Sur2p and hence trihydroxylated LCBs, Fig 5A), indicating

a preference for dihydroxylated substrates (Fig 5C) The molecular ion for the pYDESB-dependent LCB had an m⁄ z of 465, consistent with the identification of this product as a dihydroxylated long chain base of 18 carbons, containing one double bond (data not shown) The precise regiospecificity of the activity encoded by TpdesB was further investigated by comi-gration with authentic standards for desaturated dihydroxy-LCBS This indicated that the novel prod-uct present on expression of pYDESB in sur2D was not sphingosine (d18:1D4t) (Fig 5D), but instead comi-grated with the trans-isomer of d18:1D8 (Fig 5B) (as determined by coinjection with LCBs resulting from expression of the borage sphingolipid D8-desaturase in sur2D 23,24); Thus, TpdesB encodes a sphingolipidD8 -desaturase with strong preference for dihydroxylated substrates In addition, it appears that the TpDESB desaturase differs from higher plant orthologs, since it only synthesizes the trans stereoisomer of the D8 -dou-ble bond (Fig 5C, cf the stereo-unselective borage

Fig 4 GC analysis of FAMEs from yeast transformed with the

empty plasmid pYES2 or the plasmid containing TpDESK Yeast

cells transformed with either pYDESK (top chromatogram) or

pYES2 (bottom chromatogram) were induced for six days in the

presence of 22:5 D7,10,13,16,19 exogenously fed before sampling for

fatty acid analysis New fatty acid is underlined The experiment

was repeated twice and results of a representative experiment are

shown.

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sphingolipid D8-desaturase, Fig 5B) To provide

fur-ther evidence for the correct assignment of function of

TpdesB as a sphinganine D8t-desaturase, we examined

the sphingolipid LCB composition of T pseudonana

This indicated that the diatom sphingolipids are

com-posed predominantly of dihydroxylated C18-LCBs, of

which the majority are unsaturated: 76%

dienine-con-taining and 17% sphingenine-condienine-con-taining sphingolipids,

compared with 7% sphinganine-containing

sphingoli-pids Thus, 93% of T pseudonana LCBs contain one

or more double bonds

Discussion

Using a combination of molecular cloning and

bio-informatics analysis of the available T pseudonana

genome, we have been able to identify 11 putative

front-end desaturases Two lacked cytochrome b5

fusion domain and grouped with functionally

unchar-acterized putative proteobacterial desaturases Among

the remaining nine cytochrome b5 fusion domain

con-taining desaturase sequences, seven were shown to be

transcriptionally active in T pseudonana cells based on semiquantitative RT-PCR We were unable to obtain a full-length ORF for TpdesE due possibly to problems

of secondary structure in the mRNA We previously showed that despite having significant sequence similar-ity, TpDESN actually encodes aD11-desaturase specific for 16:0 and so cannot be considered as a member of the front-end desaturase functional class [18] Of the five remaining sequences we expected that at least some

if not all of these would encode desaturases involved in the biosynthesis of EPA and DHA from stearidonic acid (18:4D6,9,12,15) According to the phylogenetic ana-lysis, TpdesI, TpdesO and TpdesK were good candidates for genes encodingD6-,D5- andD4-desaturases, respect-ively Results of heterologous expression in yeast of these genes confirm these predictions TpDESI introdu-ces a double bond at position 6 from the C-terminus of endogenous 16:1D9, 18:1D9 and exogenous fatty acids 18:2D9,12 and 18:3D9,12,15 Production of 16:2D6,9 and 18:2D6,9 from yeast fatty acids has already been observed after transformation with D6-desaturase from the oleaginous fungus Pythium irregulare [25], the moss Physcomitrella patens [26], the diatoms P tricornutum [9] and higher plants [27] The fatty acid profile of

T pseudonana cells [18] suggests the existence of a

D6-desaturase that can act on 16:2D9,12 to produce the corresponding D6 fatty acid 16:3D6,9,12 TpDESI is a good candidate for this activity considering its broad substrate specificity However, we were unable to test this hypothesis by direct feeding experiments as, to our knowledge, 16:2D9,12is not commercially available TpDESO acts as aD5-desaturase on C20 fatty acids

to produce 20:4D5,8,11,14and 20:5D5,8,11,14,17as predicted from the clustering of the gene in the phylogenetic tree This enzyme is also able to introduce a double bond in

a nonmethylene interrupted pattern at the D5-position

of 20:3D11,14,17 and 20:2D11,14 but at much lower effi-ciency than the methylene interrupted pattern of activ-ity with fatty acids containing a double bond at the

D8 position The C elegans D5-desaturase was shown

to exhibit similar activities as found with TpDESO [20] The significance of this nonmethylene interrupted pattern of activity in a biological context is not clear,

as the resulting fatty acids are considered to be ‘dead end’ metabolites since they do not appear to act as precursors for signalling molecules such as prostaglan-dins and they are not present as a major fatty acid component in T pseudonana

Of the three PUFA desaturases characterized in the heterologous system, TpDESK exhibited the lowest activity with only 3.0% of 22:5D7,10,13,16,19 being desaturated to DHA Due to the low D4-desaturase activity of TpDESK on what is likely to be the

Fig 5 HPLC analysis of sphingolipid LCB profiles of yeast

trans-formed with TpdesB Total LCBs were extracted from yeast sur2D

expressing pYDESB, derivatized and separated as described (A)

LCB profile from yeast mutant sur2D which synthesizes only

dihydroxylated LCBs (e.g d18:0 ¼ dihydroxylated 18 carbon LCB,

saturated) (B) LCB profile from sur2D yeast expressing the

stereo-unselective borage sphingolipid D 8 -desaturase: note the presence

of cis and trans D 8

-desaturated dihydroxylated LCBs (inset) (C) LCB profile from sur2D yeast expressing pYDESB: note the

pres-ence of only the trans isomer of the D 8 -desaturated dihydroxylated

LCB (D) The LCB profile of pYDESB was coinjected with a

deriva-tized authentic standard for sphingosine (d18:1 D4t ): note that

sphingosine does not coelute with the novel D 8t -LCB which arises

from pYDESB expression.

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preferred substrate it is not possible to reach a

conclu-sion on the substrate preference of this enzyme for

omega-3 vs omega-6 fatty acids with the current data

TpDESI and TpDESO displayed almost no selectivity

between the omega-3 and omega-6 fatty acid

sub-strates, being equally active on both substrates

Inter-estingly the D6-desaturase is more active than the

D5-desaturase which in turn is more active than the

D4-desaturase activity of TpDESK It is not possible to

conclude if this has any significance as regards rate of

flux through these different enzymes in vivo as the

heterologous expression system could introduce

arte-facts with respect to overall activity TpDESO and

TpDESI also exhibited additional activities with

TpDESO producing 16:2D6,9 and 18:2D6,9and TpDESI

producing 20:3D5,11,14 and 20:4D5,11,14,17 However,

none of these products were detected in extracts from

T pseudonanacells [18]

An alternate pathway for PUFA desaturation has

been demonstrated in several lower eukaryotes [28]

and a gene encoding this enzyme has been isolated

from Euglena gracilis [6] In this alternate pathway, a

front end D8-desaturase acts on 20:2D11,14

(eicosadi-enoic acid) and 20:3D11,14,17 (eicosatrienoic acid) to

produce 20:3D8,11,14 and 20:4D8,11,14,17 The E gracilis

D8-desaturase is in the same subgroup as TpDESI and

TpDESE in the phylogenetic tree (Fig 1) We have

functionally characterized TpDESI in the current work

but have been unable to characterize TpDESE The

fact that we did not detect eicosadienoic acid in

T pseudonana cells, and only very low level of

eicos-atrienoic acid were measured suggests the D8

-desatu-rase alternate pathway is not present in this organism

Furthermore, acyl-CoA profiling of T pseudonana

cells, did not detect 20:2D11,14 or 20:3D11,14,17 CoA

(Tonon et al unpublished data) Therefore it is

unli-kely that TpdesE or any of the other Tpdes genes

encode a PUFAD8-desaturase

As well as the three T pseudonana cytochrome b5

fusion desaturases confirmed as front-end PUFA

desaturases, we have also identified a sphingolipid

D8-desaturase, TpDESB This is the first example of a

sphingolipid long chain baseD8-desaturase from a

mar-ine algal species It has previously been observed that

this class of sphingolipid desaturase displays a

paralo-gous relationship to the PUFA desaturases, though the

evolutionary significance of this is still unclear [29] In

that respect, the availability of the T pseudonana

gen-ome sequence may provide further insights into the

ancestry of these cytochrome b5 fusion desaturases, not

least of all as this diatom represents the first example

of an organism which carries out both front-end

LCPUFA desaturation (up to and including the

synthesis of DHA) and sphingolipid D8-desaturation However, there are several subtle difference between the TpDESB sphingolipid desaturases and the predom-inant form of the enzyme found in higher plants Firstly, TpDESB has a strong preference for dihydrox-ylated LCB substrates (i.e sphinganine), whereas almost all higher plant sphingolipidD8-desaturases dis-play greater activity towards trihydroxylated LCBs (i.e phytosphingosine) [30] A recent example of a higher plant sphingolipid desaturase with activity towards sphinganine was reported from Aquilegia vulgaris [24] The introduction of theD8-desaturation into dihydroxy-lated substrates may represent the first step in the syn-thesis of sphingadienine-containing sphingolipids (i.e containing d18:2D4t,8c⁄ t LCBs), by the subsequent

D4-desaturation of the D8-desaturated LCB This bio-synthetic route has been invoked to explain the absence

of sphingosine (i.e D4-desaturated dihydroxysphingo-sine) in many plant species, even though higher plant LCBD4-desaturases are clearly present, as witnessed by the high levels of sphinga-4,8-dienine present in plant sphingolipids Interestingly, we have detected a pre-sumptive ortholog of the dihydrosphingosine D4 -desaturase [22] in the T pseudonana genome sequence,

as well as the presence of sphingadienine LCBs (Michaelson and Napier, unpublished data) It there-fore seems likely that the biosynthesis of unsaturated sphingolipids in T pseudonana occurs in the manner initially proposed for higher plants, i.e viaD8 -desatura-tion of dihydroxy substrates, followed by D4 -desatura-tion This is in contrast to that reported for animal systems (which lack a sphingolipid D8-desaturase), where D4-desaturation occurs on an N-acylated dihy-droxylated LCB (i.e dihydroceramide) [31] Although TpDESA clustered closely to TpDESB, expression of TpDESA in either wild-type or sur2D yeast strains failed to reveal any activity as an LCB desaturase The second feature of TpDESB is that this is the first cloned example of stereo-selective sphingolipid D8 sphinganine desaturase; previous examples of the higher plant sphingolipid desaturases with this regio-specificity are stereo-unselective in terms of the double bond introduced (i.e a nonequal mixture of cis and trans configurations), though a stereo-specific D8t phy-tosphingosine desaturase has been reported from the yeast Kluyveromyces lactis [32] (see Sperling and Heinz,

2003 [30] for an excellent review of the topic of LCB desaturation) The enzymatic basis for this higher plant stereo-unselective is currently unclear, but has been hypothesized to result from a syn-elimination of two vicinal hydrogen atoms from two different substrate conformers, making this form of sphingolipid LCB desaturation distinct from the D4-desaturation which

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yields sphingosine [30] In that respect, it is perhaps

surprising to find a more ‘precise’ form of

stereo-speci-fic LCB desaturation in the unicellular diatom T

pseu-donana, which may be due to an as yet unknown role

It is also currently unclear as to the role of

sphingo-lipid LCB D8-desaturation, though it has been

hypo-thesized to be involved in chilling tolerance in some

plant species and we have observed some variation in

T pseudonanaLCB profiles according to culture

condi-tions Interestingly, the ratio of cis⁄ trans forms of D8

-desaturated LCBs in higher plants varies according to

subcellular location, with a very much enhanced level

of D8t-LCBs found in plasma-membranes and

deter-gent-resistant membranes (lipid rafts) [33] Our

obser-vation of a D8t-specific dihydroxy-LCB desaturase in

T pseudonana may therefore provide an additional

tool with which to investigate the functionality and

importance of sphingolipid LCB heterogeneity [34]

In conclusion, this comprehensive study on the

T pseudonana front-end desaturases demonstrates the

value of whole genome sequence for gene discovery

programmes Whether the complete set of PUFA

desaturases from T pseudonana represent valuable

tools for metabolic engineering of the PUFA

biosyn-thetic pathway into oil crops remains to be established

The additional activities exhibited by the D5- and

D6-desaturases could prove problematic as it would be

preferable to limit the introduced enzymatic activities

to those essential for EPA and DHA production in

order to avoid the presence of additional fatty acids in

an end product Nevertheless, this set of desaturases

along with the recently characterized D5-elongase from

the same organism represents an attractive biotechno-logical resource As highlighted in recent publications [10], a critical issue for the development of a commer-cially viable product will be the final yield of EPA and DHA in the engineered vegetable oil and this will most likely require the introduction of additional activities such as acyltransferases and acyl-CoA synthetases [35] Further mining of the T pseudonana genome should lead to identification of genes encoding these addi-tional enzyme activities

Experimental procedures

Cultivation of T pseudonana, RNA extraction and RT-PCR analysis of gene expression

T pseudonana was cultivated as described previously [18] Total RNA was extracted from cells harvested at different stages of growth using an RNeasy plant mini kit (Qiagen, Valencia, CA, USA) First-strand cDNA was synthesized from three lg of DNAse treated RNA using a Prostar First-strand RT-PCR kit (Stratagene, La Jolla, CA, USA) PCR with primer pairs specific to each T pseudonana desaturase gene (Table 1) were performed using gDNA, or undiluted and five-fold serial dilutions of cDNAs as fol-lows: the reactions were heated to 95C for 5 min followed

by 35 cycles at 95C for 30 s, 30 s at temperatures ranging between 50 and 70C according to the primer pair used and 72C for 2 min, then a single step at 72 C for 10 min The 18S rRNA gene was used to ensure that the same quantity of cDNA was used for PCR on the different RNA samples Aliquots of PCR reactions were electrophoresed through a 1% agarose gel Identity of the diagnostic

frag-Table 1 Primers used in this study Sequence of the primers is given in the 5¢ to 3¢ orientation Restriction site used for cloning in the yeast plasmid pYES2 are in bold.

RT-PCR

Yeast expression

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ment for TpdesO, TpdesM, TpdesN and TpdesG was

veri-fied by sequencing after cloning in the pGEM-T

EasyVec-tor (Promega, Madison, WI, USA)

5¢- and 3¢-RACE experiment

The GeneRacerTM kit (Invitrogen, Carlsbad, CA, USA)

was used to reverse transcribe T pseudonana RNA and

cDNA was used to amplify the 5¢-end of TpdesE and the

3¢-end of the TpdesB gene Fragments generated by nested

PCR were cloned into the pGEM-T EasyVector (Promega)

and sequenced

Functional characterization of T pseudonana

putative front-end desaturases in Saccharomyces

cerevisiae

cDNA of the entire desaturase coding region was

synthes-ized from T pseudonana RNA using the SuperScriptTMIII

RNase H– Reverse Transcriptase (Invitrogen) or the

Enhanced Avian Reverse Transcriptase (Sigma) and gene

specific primers pairs (Table 1) Forward primers for

TpdesA, TpdesB, TpdesI and TpdesO gene were designed to

contain an alanine codon (GCT) just downstream of the

start codon not present in the original algal sequences

Presence of a G at position +4 has been shown to improve

translation initiation in eukaryotic cells [36] In the case of

TpDesK, activity was detected in S cerevisiae when a full

length cDNA that did not contain the alanine codon was

used The Expand High Fidelity PCR system (Roche,

Indi-anapolis, IN, USA) was employed to minimize potential

PCR errors The amplified product was gel purified and

restricted with KpnI and SacI for TpdesA and TpdesB,

EcoRI and BamHI for TpdesI, HindIII and XbaI for

TpdesO, and BamHI and XbaI for TpdesK Each desaturase

fragment was then cloned into the corresponding sites

behind the galactose-inducible GAL1 promoter of pYES2

(Invitrogen) to yield the plasmids pYDESA, pYDESB,

pY-DESI, pYDESO, and pYDESK The fidelity of the cloned

PCR product was checked by sequencing The vectors

con-taining the T pseudonana sequences were then transformed

into S cerevisiae strain Invsc1 (Invitrogen) (or W303A1 for

pYDESK) by a lithium acetate method Transformants

were selected on minimal medium plates lacking uracil

In order to monitor LCBs sphingolipids synthesis,

pYDESA, pYDESB, pYDESI, pYDESO, and pYDESK

were also transformed into the yeast mutant sur2D

(Euro-scarf, http://www.uni-frankfurt.de/fb15/mikro/euroscarf/

index.html) As a positive control for the sphingolipid

D8-desaturation of LCBs in both WT and sur2D mutant,

the yeast expression construct containing the borage D8

-desaturase was used, as described previously [23,24]

For PUFA feeding experiment, individual transformants

were grown at 25C in the presence of 2% (w ⁄ v) raffinose

and 1% (w⁄ v) Tergitol NP-40 (Sigma, St Louis, MO, USA) Expression of the transgene was induced at D600¼ 0.2–0.3 by supplementing galactose to 2% (w⁄ v) At that time, the appropriate fatty acids were added to a final con-centration of 50 lm Incubation was carried out at 25C for 3 days and then 15C for another 3 days For the co-feeding experiment, the same conditions were applied, except that both substrates were added to 25 lm final con-centration Each feeding experiment was repeated twice, and FA analysis was carried out on triplicate samples For functional characterization of Tpdes genes in the sur2D background, cultures were grown at 22C with sha-king in the presence of 2% (v⁄ v) raffinose and induction was carried out as previously described [37] All cultures were then grown for a further 48 h unless indicated All analysis was performed on triplicate samples and replicated three times

Fatty acid analysis Microalgae or yeast cells were harvested by centrifugation Total fatty acids were extracted and transmethylated as previously described [14] Fatty acid methyl esters (FAMEs)

of methyl pentadecanoate (15:0) or methyl heptadecanoate (17:0) were included as internal standards to enable quanti-fication PUFA FAMEs were identified by comparing chro-matographic traces with transmethylated commercial Menhaden oil (Supelco, Gillingham, Dorset, UK), and by identification of picolinyl ester and dimethyl disulphide adduct structures by GCMS as previously described [18]

Sphingoid base analysis Sphingolipid analysis of yeast cells was carried out essen-tially as described previously [21] LCBs were liberated from yeast cells by alkaline hydrolysis and extracted with chloroform⁄ dioxane ⁄ water (6 : 5 : 1, v ⁄ v ⁄ v) The LCB frac-tion was converted to dinitrophenol derivatives, extracted with chloroform⁄ methanol ⁄ water (8 : 4 : 3, v ⁄ v ⁄ v), purified

by TLC on silica plates and analysed by reversed-phase HPLC using an Agilent 1100 LC system, with MS analysis carried out on a Thermoquest LCQ system with an APCI source Standards were obtained from Matreya Inc USA,

or using previously authenticated in vivo synthesized LCBs [23,24]

Acknowledgements

Financial support for this work was provided by the Department for Environment, Food and Rural Affairs grant no NF 0507 and the EU Sixth Framework Pro-gramme Integrated Project LipGene (Contract FOOD-CT-2003–505944) RQ is a visiting scholar from

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