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Báo cáo khoa học: Cooperation of two carotene desaturases in the production of lycopene in Myxococcus xanthus pot

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Noncyanobacterial bacteria and fungi use a single CrtI-type phytoene desaturase to carry out the four dehydrogenation steps producing lycopene.. We show here that the first three genes of

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production of lycopene in Myxococcus xanthus

Antonio A Iniesta1,2, Marı´a Cervantes1and Francisco J Murillo1

1 Departamento de Gene´tica y Microbiologı´a, Facultad de Biologı´a, Universidad de Murcia, Spain

2 Department of Developmental Biology, Beckman Center, Stanford University School of Medicine, CA, USA

Carotenoids constitute one of the most widely

distri-buted and structurally diverse classes of natural

pig-ments, with important functions in photosynthesis,

nutrition, and protection against photooxidative

dam-age Carotenoids are ubiquitously found in bacteria,

fungi, algae, and plants Even though the end-products

of carotenoid biosynthesis are extremely diverse, a

gen-eral common pathway leading to the formation of

lycopene (red carotene), and cyclic b-carotene (yellow)

is observed in many organisms However, the nature

of the involved enzymes varies among different

organ-isms [1] Precursors for the synthesis of carotenoids are

derived from the general isoprenoid biosynthetic

path-way (along with a variety of other important natural

substances) [2], and start with the precursor farnesyl

diphosphate (Fig 1) The condensation of two geranyl-geranyl diphosphate (GGPP) molecules produces phy-toene, mostly in the cis conformation Generally, phytoene is dehydrogenated in four desaturation events, producing phytofluene, f-carotene, neurospo-rene, and lycopene, respectively, in that order (Fig 1)

On the basis of sequence homology, there are two unrelated groups of phytoene desaturases, CrtI-like and Pds-like Noncyanobacterial bacteria and fungi use a single CrtI-type phytoene desaturase to carry out the four dehydrogenation steps producing lycopene The Pds-type phytoene desaturase is found in plants, algae, and cyanobacteria, where it is known as CrtP Both Pds and CrtP converts phytoene into f-carotene

in two steps The two remaining desaturation events

Keywords

carotenes; CrtI; dehydrogenation;

isomerization; phytoene

Correspondence

A A Iniesta, Beckman Center B355, 279

Campus Drive, Stanford, CA 94305, USA

Fax: +1 650 725 7739

Tel: +1 650 723 5685

E-mail: ainiesta@stanford.edu

F J Murillo, Facultad de Biologı´a,

Universidad de Murcia, Campus de

Espinardo, Murcia 30071, Spain

Fax: +34 957 355 039

Tel: +34 957 355 024

E-mail: francisco.murillo@juntadeandalucia.es

(Received 10 May 2007, revised 26 June

2007, accepted 28 June 2007)

doi:10.1111/j.1742-4658.2007.05960.x

In Myxococcus xanthus, all known carotenogenic genes are grouped together in the gene cluster carB–carA, except for one, crtIb (previously named carC) We show here that the first three genes of the carB operon, crtE, crtIa, and crtB, encode a geranygeranyl synthase, a phytoene desatur-ase, and a phytoene synthdesatur-ase, respectively We demonstrate also that CrtIa possesses cis-to-trans isomerase activity, and is able to dehydrogenate phytoene, producing phytofluene and f-carotene Unlike the majority of CrtI-type phytoene desaturases, CrtIa is unable to perform the four dehy-drogenation events involved in converting phytoene to lycopene CrtIb, on the other hand, is incapable of dehydrogenating phytoene and lacks cis-to-trans isomerase activity However, the presence of both CrtIa and CrtIb allows the completion of the four desaturation steps that convert phytoene

to lycopene Therefore, we report a unique mechanism where two distinct CrtI-type desaturases cooperate to carry out the four desaturation steps required for lycopene formation In addition, we show that there is a difference in substrate recognition between the two desaturases; CrtIa dehydrogenates carotenes in the cis conformation, whereas CrtIb dehydro-genates carotenes in the trans conformation

Abbreviations

CTT, casitone ⁄ Tris; GGPP, geranylgeranyl diphosphate.

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are carried out by other desaturases, Zds in plants and

algae, and CrtQ in cyanobacteria, which are related to

the Pds-type desaturases In organisms with a

CrtI-type desaturase, the cis-to-trans isomerization

convert-ing cis-phytoene into trans-phytoene is also performed

by CrtI However, the Pds-type desaturases lack

iso-merase activity, and a CrtI-like enzyme (CrtISO in

plants and CrtH in cyanobacteria) is used for

cis-to-transisomerization, converting cis-lycopene into

trans-lycopene [1] A few exceptions to these generalizations about the dehydrogenation or the isomerization pro-cess have been reported [3–7]

Myxococcus xanthus is a Gram-negative bacterium that produces carotenoids in response to blue light [8,9] and the presence of copper [10] M xanthus accu-mulates mainly esterified carotenoids such as ester of myxobacton (final carotenoids), and all-trans-phytoene (Table 1) [11,12] In M xanthus, all known and pre-dicted carotenoid biosynthesis genes are grouped together in the carB–carA gene cluster [13], except for carC (hereafter renamed crtIb) (Fig 2) [14] The first six ORFs of carB–carA are located in the carB operon, and the rest are at the carA locus We characterize here the first three genes from the M xanthus carB operon, and show that their products, CrtE, CrtIa, and CrtB, possess GGPP synthase, phytoene desatur-ase and phytoene synthdesatur-ase activity, respectively In addition, we show that M xanthus uses two

desaturas-es, CrtIa and CrtIb, to complete the four desaturation processes required to transform phytoene into lyco-pene This is the first report of such unusual and unique collaboration between two CrtI-like

desaturas-es, providing additional evidence for the wide plasticity

of carotenoid biosynthesis Finally, we also show here that CrtIa possesses cis-to-trans isomerase activity, and recognizes substrates in the cis conformation, whereas CrtIb has similar desaturase activity but recognizes substrates in the trans conformation

Results

Phytoene isomerization

In M xanthus, a mutant with a transposon insertion

in the coding region of crtIb accumulates all-trans-phy-toene (93%) and phytofluene (7%) [11] Therefore, CrtIb is required for phytoene dehydrogenation steps producing lycopene, but is dispensable for the 15-cis-phytoene to all-trans 15-cis-phytoene isomerization This sug-gests the existence of a second enzyme to carry out the phytoene isomerization and, possibly, the first phyto-ene dehydrogenation step leading to phytofluphyto-ene The product encoded by crtIa showed high similarity to the CrtI-type phytoene dehydrogenase from fungi and noncyanobacterial bacteria [13], including the previ-ously described CrtIb of M xanthus [14] An M xan-thus mutant with a transposon insertion in crtIa is unable to produce carotenoids, indicating an early role

in carotenogenesis The crtIa insertion could have a polar effect on the expression of downstream genes [12] To clarify the possible function of crtIa in the carotenoid synthesis pathway, we generated an

Fig 1 Schematic of the initial carotenoid biosynthesis pathway in

M xanthus The addition of an isopentenyl diphosphate unit (IPP)

to farnesyl diphosphate generates a GGPP molecule The

conden-sation of two GGPPs results in the synthesis of 15-cis-phytoene.

After its isomerization to the all-trans conformation, the phytoene

undergoes four dehydrogenation steps, producing phytofluene,

f-carotene, neurosporene, and lycopene, respectively Dashed

circles represent the site where the desaturation events take place.

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in-frame deletion of crtIa in M xanthus strain MR151.

This strain contains a mutation, carR3, which renders

the expression of the carB operon independent of

external stimulation [10,15] Colonies of the

MR151-derived strain with the crtIa deletion (MR841)

com-pletely lose the red color typical of colonies from the

parental strain, suggesting that the absence of CrtIa

blocks the synthesis of colored carotenoids The

possi-ble accumulation of carotenoid precursors by MR841

was analyzed by carotene extraction and

chromatogra-phy on an alumina column Only the presence of chromatogra-

phy-toene was detected (Fig 3A and Table 1) The pattern

of absorbance of this carotene is similar to that shown

by 15-cis-phytoene and different from that shown by

all-trans-phytoene (Fig 3B) Therefore, CrtIa is

required, at least, for the isomerization of

15-cis-phyto-ene to all-trans-phyto15-cis-phyto-ene

Two CrtI-type enzymes cooperate in phytoene

dehydrogenization to lycopene

In M xanthus, a transposon insertion in crtE or in

crtB of the carB operon prevents the accumulation of

Table 1 Carotenoid content of several strains of M xanthus and E coli with plasmids bearing different carotenogenic genes Mx,

M xanthus; Ec, E coli; ND, not detected.

Host Strain

Genotype (Mx)

Plasmids (Ec)

Carotenoid content (lgÆg)1of protein)a

Phytoene Phytofluene f-carotene Neurosporene Lycopene

Final carotenoids, esterified

a The average of three or more independent determinations is given b In the presence of light.

Fig 2 carB–carA gene cluster and crtIb The carB operon is transcribed by the light-inducible promoter P B and contains the first six genes of the carB–carA cluster The carA operon includes the last five genes of the cluster, and its transcription is driven by a light-independent promoter, PA.

Fig 3 The absence of CrtIa blocks the cis-to-trans isomerization

of phytoene (A) Absorption spectra in hexane of carotenoids extracted from strain MR841 (DcrtIa and carR3), showing only the presence of cis-phytoene (B) Absorption spectra in hexane of all-trans-phytoene produced by M xanthus (continuous line) and of 15-cis-phytoene produced by the fungus P blakesleeanus (dashed line), taken from Martinez-Laborda et al [11] All-trans-phytoene presents three well-defined peaks (276 nm, 286 nm, and 297 nm), unlike the spectrum of 15-cis-phytoene, which shows a maximum

at 286 nm and two inflections at 276 nm and 297 nm [46].

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carotenoids or their C40 precursors [11,12] The amino

acid sequences of CrtE and CrtB showed significant

similarities, respectively, to the GGPP and phytoene

synthase from bacteria, fungi, and plants [13] To

confirm the predicted enzyme activities of CrtE and

CrtB, the corresponding M xanthus genes were both

expressed in Escherichia coli, which lacks carotenogenic

genes E coli was transformed with a plasmid

(pFD6) harboring crtE, crtIa and crtB from the carB

operon, to generate strain FD6 In pFD6, the

expres-sion of the crt genes was under the control of the

arti-ficial constitutive promoter Part-1-2 Strain FD6 was

grown in LB medium to stationary phase, and

carote-noids were purified from the cell extract and analyzed

The absorption spectra of the extract showed the

pres-ence of all-trans-phytoene, phytofluene and f-carotene,

at decreasing concentrations (Table 1) Thus, CrtE,

CrtB and CrtIa are sufficient to carry out the synthesis

of phytoene, its isomerization, and the first two

phyto-ene dehydrogenation steps up to f-carotphyto-ene

produc-tion Similar results were obtained when crtIa was

coexpressed in E coli with the crtE and crtB genes

from Rhodobacter (data not shown) This confirms that

CrtE and CrtB have GGPP and phytoene synthase

functions, respectively, and that CrtIa, besides its

isomerase activity, is responsible for the double

dehy-drogenation of phytoene up to f-carotene CrtIa,

how-ever, seems unable to drive the rest of the desaturation

events that produce neurosporene and lycopene

As mentioned above, crtIb is somehow required for

the dehydrogenation steps converting phytoene to

lyco-pene However, the expression of crtIb in the E coli

strain producing cis-phytoene, using the crtE and crtB

genes from Rhodobacter, did not transform the initial

cis-phytoene at all (data not shown) In order to

deter-mine the specific function of CrtIb, we analyzed the

carotenoids accumulated by an M xanthus crtIb

dele-tion mutant, which also carries the carR3 mutadele-tion

(MR728) [16] MR728 was shown to accumulate

all-trans-phytoene, phytofluene, and f-carotene, in

decreas-ing concentrations (Table 1) This pattern of carotene

accumulation, notably similar to that resulting from the

heterologous expression of crtIa in E coli (strain FD6

in Table 1), indicates that CrtIb is acting at one or two

of the last dehydrogenation steps in lycopene

produc-tion, after the CrtIa isomerase and desaturase activities

The low ratio of f-carotene to phytofluene found in

both the M xanthus crtIb deletion mutant and the

E colistrain expressing crtIa indicates a low efficiency

of desaturation by CrtIa in the absence of CrtIb A

high relative accumulation of all-trans-phytoene is not

unusual, as it is also seen in an extract from an M

xan-thus wild-type strain, which, however, produces only

traces of partially desaturated phytoene products (Table 1) Altogether, the accumulated evidence sug-gests novel cooperation between two CrtI-type desatu-rases in the dehydrogenation of phytoene to lycopene

In order to determine whether both CrtIa and CrtIb are necessary and sufficient for the complete dehydro-genation to lycopene, we generated E coli strain FD9 This strain contains plasmid pFD9, which bears the

M xanthus genes crtE, crtIa, crtB and crtIb under the control of the Part-1-2 promoter Colonies from strain FD9 developed a very strong red color on LB agar plates Carotenoid analysis showed that FD9 accumu-lates high amounts of lycopene almost exclusively (Table 1) This is also seen in an M xanthus mutant defective in lycopene cyclization, where lycopene is more abundant than other desaturated precursors [12] Therefore, in M xanthus, CrtIa and CrtIb are both required to complete the four phytoene dehydrogeniza-tion steps necessary for lycopene formadehydrogeniza-tion Moreover, the exclusive accumulation of lycopene suggests some kind of cooperation between both CrtI-type dehydro-genases for the efficient processing of the partially dehydrogenated intermediate substrates

Different isomeric substrates for each dehydrogenase

The requirement in M xanthus for two CrtI-type pro-teins to carry out the four dehydrogenation steps involved in converting phytoene to lycopene is atypical

in the biogenesis of carotenoids The precise dehydro-genase activity of CrtIa and CrtIb could be due to dif-ferential substrate recognition, based on the substrate desaturation state, on its isomer conformation, or both To discriminate between these possibilities, we expressed crtIa or crtIb in E coli containing plasmid pACCRT-EBP This plasmid harbors the crtE and crtB genes from Erwinia uredovora and the gene crtP from the cyanobacterium Synechococcus PCC7942 Carotene analysis of extract from E coli with pACCRT-EBP (FD100) identified cis-f-carotene as a major carotene, and trace amounts of all-trans-f-caro-tene and cis-phytoene [5] The expression of crtIa in this strain resulted in the accumulation of the four de-hydrogenated phytoene derivatives phytofluene, f-caro-tene, neurosporene, and lycopene (FD101 in Table 1)

On the other hand, the same strain expressing crtIb produced f-carotene, neurosporene and lycopene, all in low amounts, with no phytofluene being detected (FD102 in Table 1) These data seem to indicate that CrtIa is able to carry out two consecutive dehydro-genation events on carotenes in the cis conformation: the conversion of cis-phytoene into phytofluene and

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f-carotene, and that of cis-f-carotene into

neurospo-rene and lycopene However, CrtIb appears to only

transform the small amounts of trans-f-carotene into

neurosporene and lycopene

To further confirm the hypothesis of the substrate

isomer specificity of CrtIa and CrtIb, we expressed

crtIa or crtIb in an E coli strain producing

trans-neu-rosporene [5] This strain (MR2301) contains plasmid

pACCRT-EBI bearing the crtE and crtB genes from

Er uredovora and crtI from Rhodobacter capsulatus,

which encodes a dehydrogenase that is capable of

transforming cis-phytoene into trans-neurosporene but

is unable to catalyze efficiently the fourth desaturation

step to produce lycopene The expression of crtIa

in the trans-neurosporene-producing strain did not

change the dehydrogenation state of the accumulated

carotenes (FD103 in Table 1) However, the expression

of crtIb caused the almost complete transformation of

trans-neurosporene into lycopene (FD104 in Table 1)

All of these results suggest a scenario where CrtIa and

CrtIb specific substrate recognition properties depend

on the cis–trans conformation of the substrate, rather

than on its desaturation state

Discussion

A variety of isoprenoid compounds, such as

choles-terol, dolichol, ubiquinone, coenzyme Q, isoprenoid

quinines, sugar carrier lipids, and carotenoids, are

syn-thesized by polyprenyl synthases in eukaryotic and

prokaryotic organisms Two distinct types of

evolu-tionarily conserved prenyltransferases, CrtE and CrtB,

catalyze the early reactions of carotenoid biosynthesis

from farnesyl diphosphate to phytoene [2] As

pre-dicted from sequence alignments [13], we report here

that the crtE and crtB genes from the M xanthus carB

operon encode enzymes with GGPP and phytoene

syn-thase activity, respectively After phytoene synthesis,

this carotene undergoes several desaturation events

(Fig 4) In M xanthus, an enzyme similar in sequence

to the CrtI-type phytoene dehydrogenases, previously

called CarC [11,14] and referred to here as CrtIb, was

shown to be involved in carotenoid biosynthesis The

crtIb gene is not linked to the carotenogenic carB

operon, which contains a gene predicted to encode a

second phytoene dehydrogenase [13], referred here as

CrtIa Interestingly, CrtIa is unable to catalyze the

four desaturations necessary for lycopene production

in the absence of CrtIb, and instead it leads to the

accumulation of the intermediates phytofluene and

f-carotene in decreasing amounts On the other hand,

CrtIb is itself incapable of introducing any double

bonds into phytoene We have demonstrated that a

unique collaboration between CrtIa and CrtIb is used

to successfully introduce four double bonds into phy-toene To our knowledge, this is the first case reported where two CrtI-type desaturases function together to generate lycopene

Although changes of CrtI-type enzymes producing loss or gain of dehydrogenation activities are not frequent, some cases have been reported In the bacteria

R capsulatus and R sphaeroides, CrtI introduces three double bonds into phytoene, producing neurosporene, but lacks the capacity to introduce the fourth double bond needed to produce lycopene [17,18] A fifth dehydrogenation step is carried out by a CrtI-type desaturase from the fungus Neurospora crassa, produc-ing 3,4-dihydrolycopene [19] Other variations in the lycopene biosynthesis pahtway have been reported

in some cyanobacteria species The cyanobacteria Anabaena PCC7120 converts the f-carotene produced

by CrtP into lycopene using a CrtI-type desaturase instead of the typical cyanobacterial CrtQ [5] Like

M xanthusCrtIb, the Anabaena CrtI-type desaturase is unable to introduce any double bonds into phytoene In the cyanobacterium Gloebacter, a single CrtI-type desat-urase is responsible for the four dehydrogenation steps required for lycopene formation, and homologs of crtP and crtQ are not found in its genome [6,7] It has been proposed that in the course of evolution, cyanobacteria acquired a gene encoding an unrelated CrtI-type desat-urase, which was duplicated, resulting in crtP and crtQ These two genes would be the ancestors of pds and zds from algae and plants [1] The lack of CrtP and CrtQ in Gloebacter may be related to its evolutionary distance from other groups of cyanobacteria [20] This organism

Fig 4 General representation of the pathway for synthesis of trans-lycopene from cis-phytoene and the enzymes involved in dif-ferent organisms, including M xanthus.

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is thought to retain traces of the ancestral properties of

cyanobacteria [4]

The formation of b-carotene is one of the most

com-mon steps in the synthesis of carotenoids It requires the

cyclization of lycopene to ionone end-groups Lycopene

in the cis conformation cannot be cyclized, due to its

steric arrangement, and therefore it must be synthesized

in the all-trans configuration, or be converted to that

form [1,21] In organisms that use Pds⁄ CrtP-type and

Zds⁄ CrtQ-type desaturases, where the dehydrogenation

steps are performed on carotenes in the cis

confor-mation, the final isomerization from cis-lycopene to

all-trans-lycopene is performed by a CrtI-type enzyme

called CrtISO in algae and plants, and CrtH in

cyano-bacteria [21–24] (Fig 4) cis-to-trans isomerization can

be also enhanced by light [5,25,26] However, in all

organisms that use a CrtI-type desturase, the

cis-to-trans isomerization is associated with the desaturation

processes producing trans-phytoene [6,27,28] (Fig 4)

In the case of Anabaena, the cis-to-trans isomerization

is carried out on f-carotene, instead of on phytoene, by

its CrtI-type f-carotene dehydrogenase [5] It is not clear

why two different biosynthetic pathways for lycopene

exist in nature The discovery of the biosynthetic

enzymes CrtP, CrtQ and CrtH in the green sulfur

bacte-rium Clorobium tepidum, an obligate photoautotroph,

suggests that these enzymes originated from a common

ancestor of modern-day green sulfur bacteria and

cyanobacteria [3] The fact that organisms with

CrtP⁄ CrtQ ⁄ CrtH also contain type I photosynthetic

reaction centers, and that cis carotenoids appear to

perform important functions in these reaction centers,

suggests a link between photosynthesis and the presence

of cis carotenoids [3,29] We show here that in

M xanthus, the cis-to-trans isomerization is catalyzed

by CrtIa CrtIa recognizes phytoene and also f-carotene

in the cis conformation In addition, CrtIa is unable

to dehydrogenate trans-neurosporene, indicating its

preference for carotenes in the cis conformation

However, CrtIb seems unable to recognize substrates

in the cis conformation, but can transform

trans-neurosporene into lycopene Therefore, we propose

that, in M xanthus, the whole biosynthetic process

from cis-phytoene to trans-lycopene is carried out by

the cooperation of two CrtI-type desaturases, CrtIa and

CrtIb They may form a protein complex, where CrtIa

recognizes cis-phytoene, isomerizes it to trans-phytoene,

and dehydrogenates it twice to produce

trans-f-caro-tene This last carotene would be then transferred

directly from CrtIa to CrtIb, and this desaturase would

introduce two new double bonds, forming

trans-lycopene The high water insolubility of carotenoids,

and the improvement of the desaturase efficiency of

CrtIa in the presence of CrtIb, suggest a mechanism for the direct transfer of substrates from CrtIa to CrtIb

In the absence of CrtIb, CrtIa would be blocked when bound to f-carotene The idea of a linear assembly chain for carotenoid synthesis was proposed years ago,

on the basis of work with the fungus Phycomyces blakesleeanus[30,31]

Why M xanthus uses two CrtI-type desaturases for the dehydrogenation of phytoene to lycopene is cer-tainly an unanswered question One possibility is that having two unlinked desaturase genes provides more regulatory options The crtIa gene is inserted in the carB operon, which is driven by a light-activated pro-moter [15] The expression of crtIb is also activated by light, but through a tight mechanism that operates only when the cells have reached the stationary phase

or are starved of a carbon source [14] This may have advantages if carotenoids are synthesized only when needed, in stationary phase but not before, leaving the isoprenoid components for metabolic uses in the growth phase In the presence of light, the carotenoid biosynthetic machinery would be present but blocked, waiting for the last enzymatic element, CtrIb, which reaches a very high level soon after the cell’s entrance into the stationary phase [14] This scenario would be possible if, in the course of the evolution, CrtIa lost its capacity to perform the two final desaturation steps of the four catalyzed by a typical CrtI-type enzyme, and these activities were taken over by a second desaturase, CrtIb An obvious idea is that the crtIb gene arose by duplication of the original, single M xanthus crtI gene However, the CrtIb protein is more closely related (46% identity) to the f-carotene desaturase from Anabaena PCC7120 [5] Therefore, a possible horizon-tal gene transfer event from a cyanobacterium to myxobacteria cannot be ruled out

Experimental procedures

Bacterial strains, media, and transducing phages

E coliDH5a [32] was used for cloning and carotenoid pro-duction, and E coli MC1061 [33] for transducing plasmids into M xanthus with the coliphage P1clr100Cm (hereafter called P1) [34] M xanthus strains, derived from MR151 [35], were grown in casitone⁄ Tris (CTT) rich medium [36], and E coli was grown in LB rich medium [37] When nec-essary, 40 lgÆmL)1kanamycin was added to CTT medium

Plasmid and strain construction

Standard protocols were followed for DNA manipulation [37] PCR-derived clones were generated using Pfu DNA

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polymerase, and sequenced to verify the absence of

PCR-generated mutations

To generate an M xanthus crtIa deletion mutant, we

digested plasmid pMAR161 with MluI, and the biggest

fragment was autoligated, resulting in plasmid pMAR162

Plasmid pMAR161 is a pUC9 vector [38] that contains a

4.3 kb fragment including the first three genes of the carB

operon (Fig 2) and a part of the fourth gene Plasmid

pMAR162 is similar to pMAR161 but with deletion of a

fragment encoding 160 amino acids of the coding region of

crtIa The M xanthus DNA fragment from pMAR162 was

cloned into plasmid pDAH160 [39], which carries a

kana-mycin resistance gene and the incompatibility region of P1

for transferring the plasmid from E coli to M xanthus

by P1-specialized transduction The resulting plasmid,

pMAR164, was transduced into M xanthus MR151, where

it integrated by homologous recombination to generate a

kanamycin-resistant merodiploid We grew this merodiploid

in CTT without kanamycin to allow a second

recombina-tion event that causes the loss of the kanamycin resistance

marker, generating kanamycin-sensitive colonies, either with

a wild-type crtIa or with the crtIa deletion The presence of

this deletion was confirmed by Southern blot analysis using

as a template a 4.3 kb RcaI-digested fragment from

pMAR161, and M xanthus genomic DNA digested with

NcoI The strain with the crtIa deletion was named

MR841

To make plasmid pFD3, a DNA fragment bearing crtE,

crtIa, and crtB, which also includes the ribosomal-binding

site upstream of crtE, was PCR-amplified using pMAR161

as template and the oligonucleotides ORF1-3 (5¢-GGT

TCTTCGGAGGAAAGACATATGGCACTCACGCTTCC

C-3¢) and ORF3-2 (5¢-CCGAAGCTCCGTCTAGATTCC

CTCGCCACGC-3¢) as primers The fragment was digested

by NdeI and XbaI, and cloned into the expression vector

pUC19 [40] An artificial constitutive-expression promoter,

Part-1-2, was inserted just before crtE in plasmid pFD3,

generating plasmid pFD6 and strain FD6 This promoter

was generated by hybridization of two complementary

oli-gonucleotides, Part-1 (5¢-AGCTTGACAGGCCGGAATAT

TTCCCTATAATGCGCTGCA-3¢) and Part-2 (5¢-GCG

contain the E coli RNA polymerase r70consensus binding

site, TTGACA, in position) 35 and TATAAT in position

) 10 [41], and was cloned in vectors digested with HindIII

and PstI The sequence between the) 35 and ) 10 positions

was based on the highly expressed promoter 1 of Es coli

rrnA, which encodes ribosomal RNA [42]

A DNA fragment containing the crtIb coding region plus

12 and 26 additional bp upstream and downstream,

respec-tively, was PCR-amplified using pMAR202 as a template

[14], and CRTI-1a (5¢-GTGGGATTCCGTTCATCTAGAT

ACCGGAGGGCCTTGGC-3¢) and CRTI-2 (5¢-GAGCGC

GCCACTGGATCCCGCGGCGCTCACC-3¢) as primers

The fragment obtained was cloned, after digestion with

XbaI and BamHI, into vector pUC19, resulting in plasmid pFD1 To generate plasmid pFD9 (present in E coli strain FD9), plasmid pFD1 was digested with XbaI and BamHI, and the crtIb fragment was cloned into pFD6

To generate plasmid pMAR183, a DNA fragment was amplified by PCR using pMR161 as a template, and ORF2-1 (5¢-ACCGCGCCGCCTGCAGATCCCATGAGT GCATCG-3¢) and ORF2-2 (5¢-ACCAGCGCCTTGTCGA CAGGCGGGC-3¢) as primers This fragment was digested with PstI and SalI to generate a product containing the crtIa coding region plus 2 and 14 bp upstream and downstream, respectively; this was then cloned into vector pUC9

To generate plasmid pFD39, the same crtIb fragment used for pFD9 was PCR-amplified using pMAR202 as a template, and CRTI-3 (5¢-GTGGGATTCCGTTCATCGA TATACCGGAGGGCC-3¢) and CRTI-2 as primers After digestion by ClaI and BamHI, this fragment was cloned into vector pACYC184 [43], to create plasmid pFD24 An artificial constitutive-expression promoter, Par-5-6, was inserted just before crtIb in plasmid pFD24, generating plasmid pFD26 The Part-5-6 promoter was generated

by hybridization of two complementary oligonucleotides, Part-5 (5¢-CTAGATTGACAGGCCGGAATATTTCCCTA TAATGCGCAT-3¢) and Part-6 (5¢-CGATGCGCATTAT

con-tain, like the Part-1-2 promoter, the E coli RNA polymer-ase r70 consensus binding site, and was cloned in vectors digested with XbaI and BamHI Plasmid pFD26 was digested by XbaI and BamHI, and the Part-5-6-crtIb frag-ment was cloned into vector pBJ114 [44], resulting in plas-mid pFD39

Carotenoid extraction and analysis

E coli was grown in LB medium to stationary phase, and

1 mL of this culture was inoculated into 100 mL of LB medium and incubated at 37C for 12 h FD100, FD101 and FD102 E coli strains were supplemented with isopro-pyl thio-b-d-galactoside (0.5 mm) to increase expression of crtP, and incubated at 28C for 48 h [5] In the case of

M xanthus, 100 mL of CTT was inoculated with 1 mL of culture in stationary phase, and incubated at 33C until this culture reached stationary phase Additional experi-mental procedures were identical for all cultures A 1.5 mL aliquot was taken for protein assay [15], and the remaining volume was centrifuged at 15 700 g using an Eppendorf 5415D 24-place rotor for 1.5–2.0 ml tubes (Eppendorf AG, Hamburg, Germany) to pellet the cells The pellet was stored at) 20 C until analysis

The pellet was resuspended in 20 mL of methanol by vigorous shaking for 15 min, and then centrifuged at

27 200 g using a Beckman J2-21 centrifuge and JA-20 rotor (GMI Inc., Albertville, MN, USA) and re-extracted until the sample was totally colorless An equal volume of

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light petroleum (40–60C) was added to the methanol

extract The two-phase sample was vigorously shaken for

5 min, and the upper, light petroleum phase was removed

Three further extractions with light petroleum were

per-formed, and the fractions were pooled and concentrated

under vacuum Carotenes were resuspended in 1–10 mL of

hexane, and identified by their absorption spectra and

quantified by their extinction coefficient [45] In some

cases, the concentrated extract was resuspended in 1 mL

of light petroleum and chromatographed on a Brockman

grade III deactivated alumina column [45], which was

developed using light petroleum with increasing quantities

of acetone When chromatographed in activated alumina,

the cis-phytoene accumulated by M xanthus strain

MR841 (Fig 3A) behaves like 15-cis-phytoene extracted

from the fungus P blakesleeanus, as described in detail in

Martinez–Laborda et al [11] The separated carotenes

were collected, concentrated and resuspended in hexane

for their analysis All manipulations of carotenoids were

carried out in the dark at 4C The same carotenes were

always detected in various independent analyses of the

same strain, although some quantitative differences were

observed, particularly in the heterologous expression

experiments

Acknowledgements

We thank Jose´ A Madrid for technical assistance, and

Dr Gerhard Sandmann and Dr Agustı´n Vioque for

providing plasmids and strains This work was

supported by the Spanish Ministerio de Educacio´n

y Cultura (grant PB96-1096 and fellowship to

M Cervantes), Ministerio de Ciencia y Tecnologı´a

(grant BMC2000-1006), and Fundacio´n Se´neca

(fellow-ship to M Cervantes)

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