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Tài liệu Báo cáo khoa học: Characterization and functional expression of cDNAs encoding thyrotropin-releasing hormone receptor from Xenopus laevis Identification of a novel subtype of thyrotropin-releasing hormone receptor ppt

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Characterization and functional expression of cDNAs encodingIdentification of a novel subtype of thyrotropin-releasing hormone receptor Isabelle Bidaud1, Philippe Lory2, Pierre Nicolas1,

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Characterization and functional expression of cDNAs encoding

Identification of a novel subtype of thyrotropin-releasing hormone receptor

Isabelle Bidaud1, Philippe Lory2, Pierre Nicolas1, Marc Bulant1and Ali Ladram1

1 Laboratoire de Bioactivation des Peptides, Institut Jacques Monod, CNRS-Universite´ Paris, Paris; 2 Institut de Ge´ne´tique Humaine, CNRS-UPR 1142, Montpellier, France

Thyrotropin-releasing hormone receptor (TRHR) has

already been cloned in mammals where

thyrotropin-releas-ing hormone (TRH) is known to act as a powerful stimulator

of thyroid-stimulating hormone (TSH) secretion The TRH

receptor of amphibians has not yet been characterized,

although TRH is specifically important in the adaptation of

skin color to environmental changes via the secretion of

a-melanocyte-stimulating hormone (a-MSH) Using a

dege-nerate PCR strategy, we report on the isolation of three

distinct cDNA species encoding TRHR from the brain of

Xenopus laevis We have designated these as xTRHR1,

xTRHR2 and xTRHR3 Analysis of the predicted amino

acid sequences revealed that the three Xenopus TRHRs are

only 54–62% identical and contain all the highly conserved

residues constituting the TRH binding pocket Amino acid

sequences and phylogenetic analysis revealed that xTRHR1

is a member of TRHR subfamily 1 and xTRHR2 belongs to

subfamily 2, while xTRHR3 is a new TRHR subtype

awaiting discovery in other animal species The three Xeno-pusTRHRs have distinct patterns of expression xTRHR3 was abundant in the brain and much scarcer in the peripheral tissues, whereas xTRHR1 was found mainly in the stomach and xTRHR2 in the heart The Xenopus TRHR subtype 1 was found specifically in the intestine, lung and urinary bladder These observations suggest that the three xTRHRs each have specific functions that remain to be elucidated Expression in Xenopus oocytes and HEK-293 cells indicates that the three Xenopus TRHRs are fully functional and are coupled to the inositol phosphate/calcium pathway Inter-estingly, activation of xTRHR3 required larger concentra-tions of TRH compared with the other two receptors, suggesting marked differences in receptor binding, coupling

or regulation

Keywords: thyrotropin-releasing hormone receptors; sub-types; amphibian; cloning; functional expression

Thyrotropin-releasing hormone (TRH) was first isolated

from the mammalian hypothalamus and characterized by

its ability to stimulate thyroid-stimulating hormone (TSH)

secretion [1,2] Most of the effects of TRH on the pituitary

are mediated by activation of the phospholipase C

trans-duction pathway involving a Gq-like G-protein [3] Regu-lation of TSH and prolactin secretions has also been reported in amphibians [4–6], but in this species, TRH is extremely important in the modulation of a-melanocyte-stimulating hormone (a-MSH) secretion by pituitary mel-anotrope cells of the pars intermedia [7,8] a-MSH, in turn,

is pivotal in the adaptation of skin color to environmental changes [9] TRH causes a transient increase in inositol 1,4,5-triphosphate (InsP3) formation in the pars intermedia cells of the frogs, indicating that TRH stimulates the phospholipase C pathway in melanotrope cells [10] In these cells, TRH induces also an increase of the intracellular calcium concentration [11] Amphibians also have two TRH precursors whose amino acid sequences differ by about 16% [12,13] Both contain seven copies of the TRH progenitor sequence, whereas only five TRH units are found in the rat and mouse [14,15], and six in humans [16] The 5¢-flanking region of the amphibian TRH gene lacks the regulatory sequence CAGGGTTTCC that seems to be important for regulating the thyroid hormone gene in humans [16] and rats [17]

Although TRH receptors (TRHRs) have been cloned from several species, no molecular information is presently available on the TRHR in amphibians A mouse pituitary cDNA encoding a G-protein-coupled TRH receptor (TRHR) was first isolated in 1990, using an expression cloning strategy [18] The nucleotide sequence of this receptor was subsequently used to clone TRHR cDNAs

Correspondence to A Ladram, Laboratoire de Bioactivation des

Peptides, Institut Jacques Monod, UMR 7592, CNRS-Universite´

Paris 6/7, 2 place Jussieu, 75251 Paris cedex 05, France.

Fax: + 33 1 44275994, Tel.: + 33 1 44276952,

E-mail: ladram@ijm.jussieu.fr

Abbreviations: a-MSH, a-melanocyte-stimulating hormone; EL,

extracellular loop; IL, intracellular loop; InsP 3 , inositol

1,4,5-triphos-phate; SLIC, single-strand ligation of cDNA; TM, transmembrane

domain; TRH, releasing hormone; TRHR,

thyrotropin-releasing hormone receptor; TSH, thyroid-stimulating hormone.

Proteins and enzymes: thyrotropin-releasing hormone (THYL_PIG);

releasing hormone precursor (Q62361);

thyrotropin-releasing hormone receptors (TRFR_RAT; Q9R297;

TRFR_MOUSE; Q9ERT2; TRFR_BOVIN; TRFR_SHEEP;

TRFR_CHICK; Q9DFB0; Q9DFA9); prolactin (PRL_HORSE);

thyroid-stimulating hormone (TSHB_RAT);

a-melanocyte-stimula-ting hormone (MLA_ANOCA).

Note: cDNA sequences reported in this paper have been deposited into

the EMBL database under accession numbers AJ420780, AJ420781

and AJ420782.

(Received 13 March 2002, revised 8 July 2002, accepted 30 July 2002)

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from various species, including those of rats [19–21],

humans [22–24], sheep [25], oxen [26], chickens [27] and,

more recently, fish [28], that all belong to the TRHR1

family Two cDNA isoforms of the TRHR1, generated by

alternative splicing, have been isolated from GH3

anter-ior pituitary tumor cells These two isoforms, which differ in

their C-terminal cytoplasmic tails, display no functional

differences when expressed in rat-1 fibroblasts [29]

A novel type 2 TRHR subfamily (TRHR2) was

discov-ered recently TRHR2 receptors that were 46%, 48% and

43% identical to the rat long isoform (TRHR1) have been

cloned and characterized from rats [30,31], mice [32] and fish

[28] Rat TRHR2 is more widely distributed in the brain

than is TRHR1 [33] and they differ in their agonist-induced

internalization and down-regulation/desensitization These

features suggest that they differ both functionally and

structurally [34] Rat TRHR2 is also basally more active

than TRHR1, acting via pathways mediated by the

transcription factors AP-1, Elk1 and CREB [35]

To clarify the functional significance of the TRH ligand/

receptor system in amphibians, a species where TRH has

been extensively studied and where it has particular

functions, we have described the isolation of full-length

cDNAs encoding three subtypes of the Xenopus laevis brain

TRHR (xTRHR1, xTRHR2 and xTRHR3) and their

functional expression in Xenopus oocytes and mammalian

cells We have also determined the tissue distributions of

xTRHR mRNA species by RT-PCR This study therefore

represents an important molecular landmark towards the

identification of the precise roles of TRH in amphibians

E X P E R I M E N T A L P R O C E D U R E S

Cloning and sequencing of TRH receptor cDNAs

Polyadenylated [poly(A)+] RNA isolation Three adult

male Xenopus laevis toads (CNRS, Rennes, France) were

anaesthetized by placing them on ice, killed by decapitation

and their brains immediately removed poly(A)+ RNA

(2–4 lg) was isolated from approximately 50 mg of brain

tissue using the Micro-FastTrack mRNA isolation kit

(Invitrogen)

RT-PCR analysis Degenerated oligonucleotides were

designed to conserved regions of the transmembrane

domains (TM) of several previously cloned TRHRs A first

set of primers was selected from TM1 and the end of TM6:

TGGT-3¢; TRHR-2 (antisense), 5¢-TAMGGCATCCAM

A-RMARNGC-3¢ A second one for the nested PCR was

chosen in the TM2-EL1 region and in the beginning of

TM6: TRHR-3 (sense), 5¢-TGGGTKTAYGGKTAYGT

KGGNTG-3¢; TRHR-4 (antisense), 5¢-ACMGCMARCA

TYTTMGTNACYTG-3¢ All oligonucleotides were

syn-thesized by Genset (Paris, France) The two sets of

oligonucleotide primers generated a 550-bp nested PCR

product from TRHR cDNA (see Fig 1A) Brain poly(A)+

RNA (1 lg) was reverse transcribed into cDNA using

random hexamers (20 pmol) in a volume of 20 lL

contain-ing 1X reaction buffer (50 mM Tris/HCl, pH 8.3; 75 mM

KCl; and 3 mM MgCl2), each deoxy-NTP at 0.5 mM,

ribonuclease inhibitor (0.5 U), and Moloney murine

leuke-mia virus reverse transcriptase (200 U; Clontech, Palo Alto,

CA, USA) The mixture was incubated for 60 min at 42C, heated for 5 min at 94C, and diluted with water to 100 lL

An aliquot (5 lL) of the brain cDNA mixture was amplified

by PCR in 50 lL containing 1X PCR buffer (10 mMTris/ HCl, pH 8.3; 50 mMKCl; and 1.5 mMMgCl2), 0.5 mMof each deoxy-NTP, TRHR-1 and TRHR-2 degenerated primers (0.4 lM each), and 0.2 U AmpliTaq DNA polymerase (Applied Biosystems) We used a 30-cycle program consisting of 94C for 45 s, 45 C for 1 min, and 72C for 3 min, followed by a final extension at 72 C for 10 min Five microliters of this amplified mixture was then submitted to nested PCR using more internal degen-erated primers, TRHR-3 and TRHR-4, under the same conditions The PCR products were analyzed by agarose gel (1%) electrophoresis The 550 bp amplified fragment was

Fig 1 Diagram of the xTRHR cDNA, PCR primers and PCR prod-ucts (A) Amplification of the middle region of the xTRHR cDNA by nested PCR The relative positions of the degenerated primers TRHR1, TRHR2, TRHR3, and TRHR4 are shown with the final PCR product (B) 3¢-RACE The 3¢-end amplified fragment of the xTRHR cDNA is shown The positions of the two specific oligonu-cleotide primers, TRHR5 and TRHR6, are indicated AUAP: abridged universal amplification primer (C) 5¢-SLIC xTRHR cDNA was ligated to the chemically 3¢-end modified oligonucleotide A5NV Three successive PCRs were performed using specific primers designed

to the middle region of the receptor and to the A5NV portion The resulting 5¢-end amplified fragment is shown (D) Construction of full-length xTRHR3 cDNA A fragment of the receptor starting from the 5¢-end and ending in the middle of the transmembrane domain 6 was amplified using the specific primers, TRHR10 and TRHR7, and a template corresponding to a mixture of the PCR products obtained in (A) and (C) The full-length cDNA was finally obtained using this fragment in association with the 3¢-end one and the specific primers TRHR10 and TRHR11.

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purified (Concert Rapid Gel Extraction System, Life

Technologies), cloned into the pGEM-T easy vector

(Promega Corp.) and sequenced with an ABI PRISM 377

automated DNA sequencer (Applied Biosystems Inc.,

Foster City, CA, USA) using the fluorescent dye-labeled

dideoxynucleotide method, both T7 and Sp6 primers, and

the Taq polymerase Three subtypes of brain Xenopus

thyrotropin-releasing hormone receptor were obtained and

designated xTRHR1, xTRHR2 and xTRHR3

Amplification of cDNA ends The information on the

nucleotide sequence of the cloned middle region of the

xTRHR allowed us to determine the 3¢-translated and

-untranslated regions of the brain xTRHR cDNA in

3¢-RACE experiments Two specific sense oligonucleotide

primers were designed to the TM5 and TM5-IL3 regions

of the xTRHR: TRHR-5, 5¢-CCTCTACACCCCCATT

TACTTC-3¢; TRHR-6, 5¢-CACGGTTCTGTATGGAC

TCATAG-3¢ (Fig 1B) 500 ng of brain poly(A)+ RNA

were reverse transcribed into cDNA using an

primer (5¢-GGCCACGCGTCGACTAGTACTTTTTTTT

TTTTTT-TT-3¢; final concentration: 0.5 lM, Life

Technol-ogies) in 20 lL containing 1X reaction buffer (20 mMTris/

HCl, pH 8.4; 50 mM KCl), 2.5 mM MgCl2, each

deoxy-NTP at 0.5 mM, 10 mM dithiothreitol, and SuperScript II

transcriptase reverse (200 U, Life Technologies) The

reaction was initiated by incubating the mixture at 42C

for 50 min and stopped by incubation at 70C for 15 min

and quickly placing the tubes on ice The mixture was

incubated with ribonuclease H for 20 min at 37C to

eliminate the RNA template Two microliters of this brain

cDNA mixture was then amplified by PCR under the same

conditions as for RT-PCR, using the TRHR-5 sense primer

(0.2 lM) and the antisense abridged universal amplification

primer (AUAP: 5¢-GGCCACGCGTCGACTAGTAC-3¢;

0.2 lM; Life Technologies) Two microliters of this

ampli-fied mixture was then submitted to nested PCR using the

TRHR-6 primer and the abridged universal amplification

primer, under the same conditions (Fig 1B) The PCR

products were analyzed by agarose gel electrophoresis,

purified, and cloned into the pGEM-T easy vector for

sequencing with both T7 and Sp6 primers

5¢ Single-strand ligation of cDNA [36] (5¢-SLIC)

experi-ments were performed to obtained the 5¢-translated region

of the brain xTRHR cDNA Brain Xenopus poly(A)+

RNA was extracted and reverse transcribed The cDNA

was then ligated with the 3¢-end chemically modified

oligonucleotide, A5NV (300 ng, 5¢-CTGCATCTATCTA

ATGCTCCT-CTCGCTACCTGCTCACTCTGCGTGA

CATC-NH2-3¢, Genset, Paris, France), in 11 lL containing

T4 RNA ligase (50 U, Biolabs), 1X T4 RNA ligase buffer,

and 23% polyethylene glycol The mixture was incubated at

22C for 72 h and the cDNA was purified Specific

oligonucleotide primers were designed to A5NV (A51, A52

and A53 sense primers) and to the middle region of the

xTRHR cDNA (TRHR-7, TRHR-8, and TRHR-9

anti-sense primers) Three successive PCR experiments were

performed using three sets of primers: first set, A51

(5¢-GATGTCACGCAGAGTGAGCAGGTAG-3¢)/TRHR-7

GAGACCATACAGAAC-C-3¢); second set, A52

(5¢-AGAGTGAGCAGGTAGCGAGAGGAG-3¢)/TRHR-8

GATAC-3¢) (Fig 1C) The PCR products were analyzed

by agarose gel electrophoresis, purified and cloned into the pGEM-T easy vector for sequencing xTRHR1 and xTRHR2 cDNA ends were obtained by a strategy similar

to that described above

Construction of full-length xTRHR cDNAs We used the following strategy as we were unable to amplify the full-length cDNA directly by nested PCR, probably due to the too low expression and the large size of the receptor

We used a mixture of the two partially overlapping cDNA fragments corresponding to the 5¢-region and the middle region as template for the first PCR of xTRHR3, with the oligonucleotide primers TRHR-7 and TRHR-10 (5¢-GTTTTGGGGTGGATTAAGGTAG-3¢) (Fig 1D)

An 816-bp amplified fragment was purified A mixture

of this cDNA fragment and the 3¢-region of the xTRHR3 cDNA was then used in a second PCR with the specific oligonucleotide primers TRHR-10 and

(Fig 1D) All the PCR experiments were done as described above with hybridization temperatures of 46 and 48C for the first and second PCR, respectively A 1400-bp fragment corresponding to the full-length xTRHR3 cDNA was finally purified, cloned into the pGEM-T easy vector, and sequenced in both directions using T7 and Sp6 primers

Full-length cDNAs corresponding to the xTRHR1 and xTRHR2 subtypes were amplified as described above using partially overlapping cDNA fragments and the pair of

CGTAACTTTTGCTG-3¢)/TRHR1-4 antisense (5¢-TC TGTTAAATGTACCTAAGTAGGCA-3¢) and TRHR2-2

TRHR2-4 antisense (5¢-CGACACTGTAGTAG-AGAT CACC-3¢), respectively The PCR products (xTRHR2:

1200 bp, xTRHR1: 1200 bp) corresponding to full-length cDNA were finally purified, cloned into the pGEM-T easy vector, and sequenced in both directions TRHR cDNA fragments were isolated from pGEM-T easy vector by Not1 excision and subcloned into the Not1 site of the mammalian expression vector pcDNA3.1(–) (Invitrogen) These expression vectors containing the entire coding sequence of xTRHR1, xTRHR2 and xTRHR3 were called pcDNA3.1-xTRHR1, pcDNA3.1-xTRHR2 and pcDNA3.1-xTRHR3

Voltage clamp experiments inXenopus oocytes Xenopus oocytes were isolated, prepared and maintained using standard procedures [37], and microinjected with pcDNA3.1-xTRHR1, pcDNA3.1-xTRHR2 and pcDNA3.1-xTRHR3 (approximately 10 ng of plasmid/ oocyte) Whole cell currents were measured 2 days later using a two-microelectrode voltage clamp technique (Genclamp, Axon Instruments) The activity of the

Ca2+-activated chloride channel was recorded using a standard calcium/chloride solution containing (in mM): 96 NaCl, 2 KCl, 1 MgCl2, 2 CaCl2 and 5 Hepes (pH 7.4) The holding potential was)80 mV Data acquisition and analysis were monitored by the pCLAMP7 suite (Axon Instruments)

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Calcium imaging experiments in HEK-293 cells

Human embryonic kidney (HEK-293) cells were grown to

70–90% confluence in 35 mm dishes (Nunc) in DMEM

supplemented with 10% fetal bovine serum (Eurobio) and

1% penicillin streptomycin (Gibco) One day after

trans-fection with pcDNA3.1-xTRHR, cells were trypsinized and

plated onto polyornithine-coated Laboratory-Tek

borosili-cate chambers (Nunc) and cultured for a further 24 h For

the measurement of intracellular Ca2+, cells were incubated

with 2.5 lM of the acetoxymethyl ester derivative of the

dual-excitation ratiometric Ca2+sensitive indicator fura-2

(Molecular Probes) at 37C in the dark for 30 min in Locke

buffer containing (in mM): 140 NaCl, 5 KCl, 1.2 KH2PO4,

1.2 MgSO4, 2 CaCl2, 10 glucose and 10 Hepes (pH 7.2)

Cells were then washed in Locke buffer and mounted onto

the stage of an inverted microscope (Olympus IX70)

equipped with epifluorescence optics and interfaced with

MERLINsoftware (LSR, Cambridge UK) to a

monochro-mator (Spectramaster) and a 12/14 bit frame transfert rate

digital camera (Astrocam).MERLINsoftware was also used

to calculate the 340/380 fluorescence ratio (Rf) The

intensity of fluorescent light emission (k¼ 510 nm) using

excitation at 340 and 380 nm was monitored for each single

fura-2 loaded cell in the field TRH (1 lMand 10 lM) and

ATP (10 lM) were prepared freshly in Locke buffer

and placed close to the cells studied Data are presented

as mean ± SEM, and n is the number of cells used

Student’s t-test was used for statistical analysis

RT-PCR distribution of xTRHR mRNAs

Poly(A)+RNA was isolated from the brain, heart, liver,

ventral and dorsal skin, testis, stomach, intestine, urinary

bladder and lungs of adult male Xenopus laevis toads

Poly(A)+RNA extracted from rat testes and ovaries were

used as positive and negative controls, respectively

RT-PCR experiments were performed under the same

condi-tions described for the RT-PCR analysis (oligonucleotide

primers: TRHR-1/TRHR-2 and TRHR-3/TRHR-4; length

of the amplified fragment: 550 bp) The poly(A)+RNA

preparations were checked for contamination with genomic

DNA by treating each mRNA sample with and without

reverse transcriptase before the PCR reactions The PCR

products were analyzed by agarose gel electrophoresis The

purified 550 bp fragments from the positive tissues were

cloned into the pGEM-T easy vector and sequenced The

amounts of TRHR mRNA in these tissues were compared

using a set of oligonucleotide primers corresponding to the

XenopusEF1a elongation factor that generates an

approxi-mately 280 bp product as an internal control

Phylogenetic analysis

The nucleotide sequence of TRH receptors from humans

(GenBank accession number NM_003301), sheep (X95285),

oxen (D83964), rats (NM_013047, AF091715), mice

(NM_013696, AF283762), chickens (Y18244) and the

teleost fish Catostomus commersoni (AF288367,

AF288368) were obtained from GenBank The nucleotide

sequences of the TRHR transcripts were aligned with

CLUSTAL W

3 [38] and by eye Molecular phylograms from the

alignment were determined with the maximum likelihood

methods in Phylip [39] Distance methods and parsimony methods were also used and gave similar results Levels of support for branches were estimated with bootstrapping methods (500 replicates) and withPHYLIP

R E S U L T S Cloning of xTRHR cDNA subtypes from Xenopus laevis brain RT-PCR experiments were performed using brain Xenopus laevismRNA as template and degenerated oligo-nucleotides designed to the conserved regions of transmem-brane domains of several TRHR cloned in mammalian species Since no signal was obtained after a first PCR, a second PCR was realized with more internal oligonucleotide primers A 550-bp amplified fragment (Fig 1A) was ligated into the cloning pGEM-T easy vector Screening of 18 subclone fragments by DNA sequence analysis revealed three distinct TRHRs, xTRHR3, xTRHR2 and xTRHR1 Their relative abundances were xTRHR3 xTRHR2 > xTRHR1 The nucleotide sequence of these partial cDNAs were only 63–65% identical (xTRHR3/2: 63%; xTRHR3/1: 65%; xTRHR2/1: 64%), while their deduced amino acid sequences were 56–66% identical (xTRHR3/2: 58%; xTRHR3/1: 66%; xTRHR2/1: 56%)

5¢ and 3¢ amplification of cDNA ends (see Experimental procedures, Fig 1B,C) gave the full-length cDNAs of these TRHR subtypes (Fig 2) The sequence of xTRHR3 contained a 1215-bp open reading frame encoding a protein

of 404 amino acid residues with a theoretical molecular weight of 45.5 kDa Hydropathy analysis using the Kyte and Doolittle algorithm [40], predicted seven transmem-brane domains, in agreement with the topology proposed for other G protein-coupled receptors [41] The deduced amino acid sequence contained three potential sites for N-linked glycosylation (N-X-S/T) in the N-terminus at positions 3, 14 and 19 (Fig 3) Interestingly, Asn19 also represents a potential glycosylation site that is absent in mammalian and chicken TRH receptors The glycosylation site in EL2 (extracellular loop 2) of the mammalian receptor was not found in xTRHR3, as for chicken TRHR The amphibian receptor had several amino acids that are highly conserved in mammals These included all the putative residues that interact with TRH (Tyr113, Asn117, Tyr287 and Arg311), and the two Cys residues (105 and 186) that form a disulfide bond between EL1 and EL2 to maintain the receptor in a high affinity conformational state Several Ser and Thr residues were also present in the C-terminus and IL3 (intracellular loop 3) regions of the Xenopus receptor These may be sites for phosphorylation by protein kinases However, only one of the two homologous Cys residues that may be palmitoylated in the mouse receptor was found in the C-terminal tail of xTRHR3 (Cys342)

The complete nucleotide sequences of xTRHR2 and xTRHR1 were obtained with the same strategy as that used for xTRHR3 The nucleotide sequences of the translated region of xTRHR2 (1206 bp) and xTRHR1 (1194 bp) cDNAs are shown in Fig 2 These sequences encode a seven transmembrane domain protein of 401 amino acids (45.2 kDa) for xTRHR2 and 397 amino acids (45.0 kDa) for xTRHR1 Alignment of the deduced amino acid sequences with that of xTRHR3 (Fig 3) showed that xTRHR2 and xTRHR1 contained most of the amino acid residues that are conserved in other TRH receptors, but

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differed in several respects from xTRHR3 xTRHR1 had

only two potential sites for N-linked glycosylation in its

N-terminus, at the conserved positions (3 and 10), while

xTRHR2 had these sites at positions 3 and 12 The

glycosylation site in EL2 (Asn167 for xTRHR1 and Asn172

for xTRHR2) and the two homologous Cys residues (335

and 337 for xTRHR1, 339 and 341 for xTRHR2) in the

C-terminal tail were also found

The three Xenopus TRHR subtypes were found to be

only 54–62% identical (62–63% for the nucleotide

se-quence) The N-termini, the IL3, and the C-termini of the

three Xenopus subtypes contained important differences,

and were only 16–30% (N-term), 25–47% (IL3) and 27–

40% (C-term) identical (Table 1) These regions also

differed markedly from the known TRH receptors,

especi-ally xTRHR3 and xTRHR2 This is particularly interesting

considering the functional importance of the third

intracel-lular loop and the C-terminal tail in receptor coupling and

regulation The amphibian EL1, IL1, IL2, and EL3 regions

were only 53–80%, 67–100%, 62–87%, and 50–80%

identical to those of mammalian TRHR1, whereas these

regions of the mammalian type 1 receptors are identical

xTRHR2 was 63% identical to mouse TRHR2, 57%

identical to the rat TRHR2, and 51% identical to fish

TRHR2 However, if the most divergent regions of the

xTRHRs (i.e N-term, IL3 and C-term) are excluded,

xTRHR2 seems to belong to the TRHR subfamily 2 because it is significantly similar to the rat, mouse and fish TRHR2 in EL1 (73–87% identity), EL2 (64–68%), EL3 (50–70%), IL1 (50–83%), and IL2 (81–94%) xTRHR1 is closer to the TRHRs subtype 1 with 66–78% identity Our data indicate that xTRHR3 is only 58–62% identical to the TRHR1 family (including xTRHR1) and only 54%, 47%, 61% and 43% identical to the Xenopus, rat, mouse and fish TRHR2s This observation, plus the fact that the sequences most similar to xTRHR3 found in the data banks were TRHRs, suggested that xTRHR3 is a novel TRHR subtype

Functional expression of xTRHR subtypes in Xenopus oocytes and HEK-293 cells The xTRH receptors were expressed in Xenopus oocytes and the mammalian

HEK-293 cell line (Figs 4 and 5) Oocytes injected with xTRH receptor cDNA 2 days previously showed a typical Ca2+ -dependent Cl–current when the bath contained 1 lMTRH (Fig 4A) This inward current consists of a large, rapid and transient response that is typical of Ca2+-dependent Cl– channels activated after stimulation of PLC and the subsequent InsP3-dependent mobilization of Ca2+ from intracellular stores Control oocytes not injected with pcDNA3.1-xTRHR (data not shown) gave no response Several TRH concentrations (0.01–10 l ) were also tested

Fig 2 Nucleotide sequence of the three Xenopus TRHR cDNA subtypes The alignment ( CLUSTAL W )

ATG is shown Asterisks (*) indicate identical nucleotides between the three cDNA sequences.

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Since TRH desensitized the receptor (data not shown), one

dose of TRH was tested and the maximum current

amplitude of each recording was measured and reported

as a function of the TRH concentration (Fig 4B) The

average dose–response profiles showed differences between

the three xTRHR subtypes, with oocytes expressing

xTRHR3 cDNA giving a particularly poor response to

0.1 lM and 1 lM TRH Similar studies in mammalian

HEK-293 cells confirmed that Xenopus TRH receptors

acted via the phosphoinositide-calcium transduction

path-way (Fig 5) TRH (1 and 10 lM) did not activate a Ca2+

transient in control cells not transfected with xTRHR

cDNA, while ATP (10 lM), which activates P2Y receptors

[42], produced Ca2+transients in living cells The responses

of HEK-293 cells transfected with the three xTRHR

subtypes differed in the same way as the transfected oocytes

One micromolar TRH did not trigger Ca2+transient in cells

transfected with pcDNA3.1-xTRHR3, whereas the same

TRH dose produced a Ca2+response in cells expressing

xTRHR2 and xTRHR1 cDNAs

Distribution of xTRHRs The distributions of xTRHRs in

the brain, liver, testis, urinary bladder, stomach, ventral and

dorsal skin, lung, heart and intestine were also examined

No signal was obtained by Northern blotting, probably

because there was too little of the Xenopus receptors, so we

used RT-PCR (Fig 6) The cDNA from each organ was

amplified using the two sets of degenerated primers

(TRHR-1/TRHR-2 and TRHR-3/TRHR-4) that gave us

the middle portion of the xTRHRs (Fig 1A) The expected

fragment was found in the rat testis (positive control) but

not in the rat ovary (negative control) (Fig 6A) No signal

was detected in the absence of the cDNA template (data not shown) A 550-bp amplified product was observed in all the Xenopustissues tested except the liver and the ventral skin The amount of the xTRH receptor mRNAs in these tissues was assayed using a set of primers corresponding to the XenopusEF1a elongation factor cDNA as internal control (Fig 6B) The highest concentration of xTRHR mRNA was detected in the Xenopus brain, with a considerable amount in the intestine (Fig 6C) Similarly strong signals were obtained in the lung and heart, with a smaller signal in the testis There was much less TRHR mRNA in the urinary bladder and stomach The xTRHR subtypes were identified by purifying the 550-bp PCR product from all the Xenopustissues, cloning them in the pGEM-T easy vector, and sequencing Sequence analysis of numerous clones indicated that the three xTRHR subtypes were present in the brain (18 clones tested: four xTRHR1, five xTRHR2 and nine xTRHR3), heart (22 clones: one xTRHR1, 17 xTRHR2 and four xTRHR3), and stomach (14 clones: nine xTRHR1, three xTRHR2 and two xTRHR3) Only xTRHR1 was present in the lung (11 clones tested), the intestine (three clones) and the urinary bladder (four clones) However, the two other subtypes could be present in these tissues We have also detected xTRHR1 and xTRHR2 in the testis and xTRHR1 in the dorsal skin

D I S C U S S I O N TRH is a powerful stimulator of TSH secretion by the anterior pituitary cells of mammals, but this function is less clear in amphibians, where TRH seems to be implicated in regulating a-MSH, thus controlling the adaptation of skin

Fig 3 Comparison of the deduced amino acid

sequences of the three Xenopus TRHRs The

alignment was prepared using CLUSTAL W

Asterisks (*) indicate residues identical in the

three subtypes Putative transmembrane

domain helixes (bold letters) were assigned

based on those of the previously cloned TRH

receptors Arrows indicate the residues (Y106,

N110, Y282 and R306) that are highly

con-served in the other TRHRs and that interact

directly with TRH The additional potential

glycosylation site (Asn19) in the N-terminus

and the absence of the homologous Cys335

(Arg340) in the C-tail of xTRHR3 are

indi-cated in gray background The non

conven-tional putative phosphorylation sites of

xTRHR1 (cAMP/cGMP-dependent protein

kinase) and xTRHR2 (tyrosine kinase) are

indicated with dashed and solid lines.

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color to changes in the environment To obtain further

information on the way TRH acts in this species,

charac-terization of TRH receptors is necessary Therefore, in this

study, we provide the first molecular characterization of

several TRH receptors from Xenopus laevis (xTRHRs) We

have cloned and functionally expressed three distinct

xTRHR subtypes The specific functional properties of the

recombinant xTRHRs have been analyzed in Xenopus

oocytes and HEK-293 cells We also report on the

distribution profiles of the xTRHR mRNAs

We used a degenerate PCR cloning strategy to isolate

three distinct subtypes of TRHR cDNA (xTRHR1,

xTRHR2 and xTRHR3) from Xenopus brain These encode

the entire sequences of the proteins The amino acid

sequence of xTRHR1 is very similar (74–78% identity) to

that of its mammalian subtype 1 counterparts, indicating

that it is a member of the type 1 TRHR subfamily The

dissimilarity between xTRHR2 and the two other Xenopus

TRHRs and its similarity to most of the regions of the mouse, rat and fish TRHR2 indicate that xTRHR2 is a member of the recently described TRHR subfamily 2 xTRHR3 corresponds to a novel TRHR subtype that is only 58–62% identical to the TRHR1 family, including xTRHR1, and only 54%, 47%, 61% and 43% identical to the Xenopus, rat, mouse and fish TRHR2s

We analyzed the molecular evolution of TRHR tran-scripts from various animal species to identify the origins of the TRH receptor subtypes The molecular phylogram of TRHR sequences is not completely resolved, but two distinct clades are apparent (Fig 7) Sequences from human, sheep, ox, rat, mouse, chicken and Xenopus type 1

Table 1 Amino acid identities in the various portions of the three

TRHRs subtypes and comparison with a lower vertebrate (fish) and a

mammal (mouse) containing both TRHR type 1 and type 2 Percentage

identities were calculated by CLUSTAL W

% identitya

N-term

EL1

EL2

EL3

IL1

IL2

IL3

C-term

a X1, X2, X3, Xenopus TRHR subtype 1, 2 and 3; M1, mouse

TRHR1 (NM_013696); M2, mouse TRHR2 (AF283762); F1, fish

TRHR1 (AF288367); F2, fish TRHR2 (AF288368).

Fig 4 Functional expression of xTRH receptors in Xenopus oocytes (Upper) Typical Ca2+-activated Cl– current traces obtained in xTRHR3 (upper trace), xTRHR2 (middle trace) and xTRHR1 (bot-tom trace) cDNA injected oocytes Xenopus oocytes were constantly perfused with ND96 solution and TRH (1 l M ) was applied to oocytes for 30 s Note the fast desensitization of the responses (Lower) Responses of the three xTRHR subtypes to different concentrations of TRH The maximum current amplitude of each recording was meas-ured and reported as a function of TRH concentration The white star indicates the average value and n represents the number of oocytes tested for each condition.

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TRH receptor cluster tightly together, suggesting that they

represent orthologous loci in these species A second clade

of orthologous sequences consists of type 2 TRH receptors

from rat, mouse, fish and Xenopus As shown in the

phylogram, the TRHR sequences do not cluster according

to animal species This pattern implies that type 1 and type 2

TRH receptors loci originated in a common ancestor prior

to the divergence of the species sampled and that concerted

evolution has played a very small role in the evolution of this

gene family The relationships of type 3 and type 2 TRHRs

from Xenopus in the second clade suggest that these two loci

are not the result of duplication of a Xenopus gene, but that

the type 3 receptor originated in the common ancestor of

fish and amphibian Although this particular locus may now

be extinct in fishes and mammals, it is more likely that the

type 3 receptor is awaiting discovery in these species

The putative binding pocket identified in the

transmem-brane domains of the mouse receptor is completely

conserved in the three Xenopus TRHR subtypes (Fig 3)

The candidate residues interacting directly with TRH are

Tyr106 and Asn110 in TM3, Tyr282 in TM6, and Arg306 in

TM7 (in Xenopus and mouse TRHR1) [41] Tyr106 and Asn110 have been reported to form hydrogen bonds with the pyroGlu residue of TRH and Arg306 with the ProNH2

Fig 5 Ca2+imaging experiments on HEK-293 cells expressing xTRHR

subtypes We measured the change in Ca2+concentration was

exam-ined in HEK-293 cells loaded with fura-2 and evaluated from the ratio

of fluorescence at 340 nm and 380 mm (Rf 340/380) The average

amplitude of the response of each cell was estimated by the ratio rF max /

rF min , where rF max corresponds to maximum Rf 340/380 during the

drug application, and rF min corresponds to Rf 340/380 just before drug

application The change in the ratio Rf 340/380 during application of

TRH (1 and 10 l M ) and ATP (10 l M ) is shown with the corresponding

average rF max /rF min ratios for the control and the cells expressing the

different xTRHR subtypes.

Fig 6 RT-PCR distribution of Xenopus TRHR in various tissues (A) Amplification of the middle portion of xTRHR cDNA (550 bp) using the two sets of degenerated oligonucleotide primers, TRHR-1/ TRHR-2 and TRHR-3/TRHR-4 (see Fig 1A) PCR products were analyzed by agarose gel (1%) electrophoresis (B) Amplification of cDNA templates with a set of primers corresponding to the Xenopus EF1a elongation factor cDNA (280 bp) as internal control of the poly(A) + RNA (C) Tissue comparison of the level of expression of xTRHRs with samples containing the same total quantity of mRNA The cDNA templates used were from: Xenopus liver (3), brain (lane 4), testis (lane 5), urinary bladder (lane 6), stomach (lane 7), lung (lane 8), heart (lane 9), intestine (lane 10) and dorsal skin (lane 11) Rat testis (lane 1) and ovary (lane 2) were used as positive and negative controls, respectively.

Fig 7 Molecular phylogram of nucleotide sequences of TRH receptor transcripts reconstructed by maximum likelihood methods Type 1 TRH receptor from the teleost fish Catostomus commersoni was the most basal sequence and was used to root the tree Bootstrap values from

500 replicates greater than 50% are indicated at nodes.

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residue Tyr282 was reported to interact hydrophobically

with the imidazole ring of TRH Other residues are highly

conserved in the three Xenopus TRH receptors These

include the two Cys residues 98 and 79 (in Xenopus and

mouse TRHR1), said to form a disulfide bond between EL1

and EL2 to maintain the TRH receptor in a high-affinity

conformational state [43] The residues Asp71 and Arg283

that are necessary for receptor activation [44,45] are also

present These residues are thought to form ionic or

hydrogen bonds with other TM residues to keep the

receptor in the active conformation after TRH binds

Altogether these data indicate that these novel G

protein-coupled receptors are clearly TRH receptors

An important finding of this study is the description of a

novel TRH receptor subtype that does not belong to the

subtypes 1 and 2 of TRHR This xTRHR3 subtype has

several distinctive features This is the only TRH receptor

that contains an additional potential glycosylation site in the

N-terminus (Asn19) xTRHR3 lacks the glycosylation site

in EL2, as do the chicken, fish (type 1 and 2), rat (type 2)

and mouse (type 2) TRH receptors Glycosylation may play

a role in the receptor expression or stability [46] Another

feature of TRHRs is the presence of two Cys residues in

their C-terminal tails that are observed in xTRHR1 (Cys335

and 337) and xTRHR2 (Cys339 and 341) By contrast, only

one of these residues (Cys342) corresponding to the

homologous Cys337 is present in xTRHR3 (also in fish

TRHR2) Since palmitoylation of homologous Cys may be

necessary for optimal interaction with the internalization

machinery [47], it is tempting to suggest that xTRHR3

might be differently processed in the cell machinery The

C-terminal region of the chicken and mammalian TRHR1

contains another residue, Phe363 (in mouse TRHR1),

which may be important in signaling endocytosis [3] This

residue is present at position 369 in xTRHR1 but is not

found in the two other Xenopus TRHR subtypes; it is also

absent from fish TRHR1 and rat, mouse and fish TRHR2

There are unconventional putative phosphorylation sites

in the Xenopus TRH receptors The C-terminal tail of

xTRHR1 contains a putative phosphorylation site for

cAMP/cGMP-dependent protein kinase (R/K-R/K-X-S/T)

at position 339 (KKRS); this is also found in fish TRHR1,

but in IL3 (KKDS at position 235) xTRHR2 contains a

putative tyrosine kinase phosphorylation site (R/K-XX or

XXX-D/E-XX or XXX-Y) in the C-tail (KAGPEGDLY at

position 389) xTRHR2 also has two putative casein kinase

II phosphorylation sites that are not found in IL3 of the

TRH receptor (also one in fish TRHR2) Altogether these

data greatly contribute to the understanding of the

molecular blueprint of the Xenopus TRH receptors and

further indicate that differential regulations of the xTRHR

subtypes may participate to their physiological functions

RT-PCR analyses showed that the TRH receptors are

present in the central and peripheral tissues of Xenopus

laevis An in situ hybridization study is in progress to

accurately determine the anatomical distribution of the

three xTRHR subtype mRNAs in the Xenopus brain

Previous studies revealed that mammalian TRHR2 is more

widely distributed in the central nervous system than is

TRHR1 [30,33,34], suggesting that TRHR2 mediates many

of the known functions in the brain that are not transduced

by TRHR1 In the Xenopus peripheral tissues, the intestine

contains the highest concentration of xTRHR mRNA The

heart and the stomach contain the three xTRHRs, but xTRHR2 is most abundant in the heart and xTRHR1 in the stomach We also found xTRHR1 and xTRHR2 in the testis and xTRHR1 in the dorsal skin Interestingly, xTRHR3 is weakly expressed in the peripheral tissues, while xTRHR1 seems to be specific to the intestine, lung, and urinary bladder The physiological functions mediated

by the three Xenopus TRHR subtypes in the central nervous system and in the peripheral tissues remain to be elucidated Using functional expression strategies, we finally demon-strate that the three xTRHRs are fully functional when expressed either in Xenopus oocytes or in mammalian HEK-293 cells Typical Ca2+-dependent Cl–currents were recorded when TRH was added Xenopus oocytes expressing xTRHRs Similarly, in transfected HEK-293 cells, a TRH-induced intracellular Ca2+ response was also observed, indicating that the Xenopus TRH receptors are coupled to the PLC/ InsP3 pathway All three receptors produced a rapidly desensitizing response following TRH application Interestingly, activation of xTRHR3 in both Xenopus oocytes and mammalian cells required larger concentrations

of TRH to produce Ca2+-dependent responses comparable

to those produced by xTRHR1 and xTRHR2 This lower response is probably not due to the vector itself since the response of the two other subtypes would also be affected, suggesting rather for xTRHR3 a lower stability or affinity for TRH Although our results indicate that xTRHR3 contains all the structural characteristics of the TRHR receptors, we effectively cannot exclude that xTRHR3 is an orphan receptor Pharmacological experiments will be necessary to assess if the weak effect of TRH observed for xTRHR3 corresponds to a low expression (Bmax) or affinity (Kd) Current work is in progress to elucidate these issues Overall, this study demonstrates that expression of distinct TRH receptors can account for the specific features

of the TRH signaling in Xenopus oocytes and further suggests the existence of a third TRHR subtype that has yet

to be identified in other species

A C K N O W L E D G M E N T S

The authors thank Drs J Moreau and T Foulon for their expert assistance, and Dr M.C Gershengorn for a critical reading of this manuscript This work was funded entirely by the Centre National de la Recherche Scientifique (CNRS).

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