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Báo cáo khoa học: Identification and characterization of a collagen-induced platelet aggregation inhibitor, triplatin, from salivary glands of the assassin bug, Triatoma infestans ppt

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Here, we describe two major salivary proteins, triplatin-1 and -2, from the assassin bug, Tria-toma infestans, which inhibited platelet aggregation induced by collagen but not by other a

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platelet aggregation inhibitor, triplatin, from salivary

glands of the assassin bug, Triatoma infestans

Akihiro Morita1, Haruhiko Isawa2, Yuki Orito1, Shiroh Iwanaga3, Yasuo Chinzei1and Masao Yuda1

1 Department of Medical Zoology, School of Medicine, Mie University, Edobashi, Tsu, Japan

2 Department of Medical Entomology, National Institute of Infectious Diseases, Toyama, Sinjyuku-ku, Tokyo, Japan

3 Laboratory of Chemistry and Utilization of Animal Resources, Faculty of Agriculture, Kobe University, Hyogo, Japan

Injury to the blood vessel wall exposes the

subendo-thelial extracellular matrix, which is rich in collagens,

providing a substrate for platelet adhesion and

aggre-gation This is the first step of hemostasis ending in

formation of the thrombus Several proteins on the

platelet membrane participate in collagen–platelet

interactions in a direct or indirect manner [1]

Glyco-protein (GP)VI [2–5] and a2b1 integrin [6] bind to

col-lagen directly, and GPIb-V-IX [7] and aIIbb3 integrin

[6,8] bind via von Willebrand factor (vWF) In the

cur-rent ‘two-site, two-step’ model of platelet–collagen

interaction [9–12], platelet aggregation proceeds as

fol-lows: first, GPIb-IX-V rapidly binds to vWF

immobi-lized on collagen so that passing platelets are tethered

to the latter Following this event, GPVI, a surface

signaling receptor, binds to collagen with low affinity,

which triggers the signaling cascade for platelet activa-tion This leads to ‘inside-out’ activation of a2b1 and

aIIbb3 integrins and secretion of platelet agonists such

as ADP and thromboxane A2, accelerating platelet aggregation and thrombus formation Therefore, GPVI has a central role in the initial phase of thrombus for-mation as the major signaling receptor for collagen GPVI is composed of two extracellular immunoglob-ulin domains, a mucin-rich stalk, a single transmem-brane domain, and a short cytoplasmic tail [2–4] GPVI is coupled to the Fc receptor (FcR) c-chain homodimer in the transmembrane domain via a salt bridge [5,9,10,13,14] The binding of collagen to GPVI leads to cross-linking of GPVI molecules [15], inducing tyrosine phosphorylation of the cytoplasmic tail of FcR c-chains This phosphorylation leads to binding

Keywords

collagen-induced platelet aggregation

inhibitor; triplatin; Triatoma infestans

Correspondence

M Yuda, Department of Medical Zoology,

School of Medicine, Mie University,

Edobashi, Tsu, Mie 514–8507, Japan

Fax: +81 59231 5215

Tel: +81 59231 5013

E-mail: m-yuda@doc.medic.mie-u.ac.jp

(Received 1 March 2006, revised 19 April

2006, accepted 4 May 2006)

doi:10.1111/j.1742-4658.2006.05306.x

To facilitate feeding, certain hematophagous invertebrates possess inhibi-tors of collagen-induced platelet aggregation in their saliva However, their mechanisms of action have not been fully elucidated Here, we describe two major salivary proteins, triplatin-1 and -2, from the assassin bug, Tria-toma infestans, which inhibited platelet aggregation induced by collagen but not by other agents including ADP, arachidonic acid, U46619 and thrombin Furthermore, these triplatins also inhibited platelet aggregation induced by collagen-related peptide, a specific agonist of the major colla-gen-signaling receptor glycoprotein (GP)VI Moreover, triplatin-1 inhibited

Fc receptor c-chain phosphorylation induced by collagen, which is the first step of GPVI-mediated signaling These results strongly suggest that trip-latins target GPVI and inhibit signal transduction necessary for platelet activation by collagen This is the first report on the mechanism of action

of collagen-induced platelet aggregation inhibitors from hematophagus invertebrates

Abbreviations

CRP, collagen-related peptide; FcR, Fc receptor; GP, glycoprotein; MBP, maltose-binding protein; PGE1, prostaglandin E1; PRP, platelet-rich plasma; vWF, von Willebrand factor.

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and subsequent activation of the tyrosine kinase, Syk,

which initiates downstream signaling events [16]

Various platelet inhibitors are found in

hematopha-gus invertebrates [17,18] These inhibitors interfere

with platelet aggregation in host animals and facilitate

blood feeding They include inhibitors of

collagen-sti-mulated platelet aggregation, but only a small number

of inhibitors of this type have been characterized

LAPP [19–21] and calin [22] were identified from

Haementeria officinalisand Hirudo medicinalis,

respect-ively They prevent both the binding to collagen of

a2b1and the binding of GPIb-IX-V to vWF, inhibiting

platelet aggregation and platelet adhesion to collagen

Moubatin [23,24] and pallidipin [25] were identified

from Ornitohdoros moubata and Triatoma pallidipennis,

respectively These proteins inhibit platelet aggregation

induced by collagen, but not platelet adhesion to

colla-gen under static conditions However their inhibitory

mechanisms and target molecules remain unknown

Here, we have identified the novel platelet

aggrega-tion inhibitors triplatin-1 and -2, from T infestans

They share sequence similarity with pallidipin and

spe-cifically inhibit platelet aggregation induced by

colla-gen We suggest that triplatins target GPVI and block

platelet activation induced by collagen

Results

Cloning and production of triplatin-1 and -2

recombinant proteins

A cDNA library was constructed from the salivary

glands of unfed T infestans Five hundred and fifty

clones were randomly picked from this library and

sequenced Among them, the most abundant species

(25 clones) corresponded to a cDNA encoding a 178

amino acid protein with a molecular mass of

19.5 kDa In addition, an isoprotein of this abundant

clone (four additional clones) was also found This

iso-form contains 182 amino acids with a molecular mass

of 19.8 kDa Both molecules were predicted to be

secretory proteins by the signal p program, and both

shared sequence similarities with pallidipin, a platelet

inhibitor found in T pallidipenis (Fig 1) Identities of

the abundant clone and its isoprotein with pallidipin

are 63 and 49%, respectively We named this salivary

gland protein and its isoprotein ‘triplatin-2’ and

‘trip-latin-1’, respectively

To investigate the function of these triplatins,

recombinant proteins were produced in a

baculovirus-insect cell system Secreted recombinant proteins

formed a major fraction of all the proteins in the

cell culture medium They were purified by

cation-exchange and gel filtration chromatography Purity was confirmed by SDS⁄ PAGE (Fig 2) Apparent molecular masses of purified recombinant triplatin-1 and -2 were approximately 17 kDa on SDS⁄ PAGE, which agreed with their predicted molecular masses of 17.9 and 17.1 kDa in secreted form

To identify native proteins in the saliva, antisera were raised against recombinant triplatin-1 In western blot analysis, the sera reacted with both triplatin-1 and -2, although relatively weakly with the latter (Fig 2) The sera also reacted with native proteins in salivary glands, showing that both triplatin-1 and -2 are indeed expressed there SDS⁄ PAGE and western blot analysis indicated that triplatin-1 and -2 are major proteins of

T infestanssaliva

Fig 1 Alignment of triplatin-1 and -2 sequences Multiple align-ment of triplatin-1 and -2 sequences with pallidipin from T pallidi-pennis by CLUSTAL W Underlining, asterisks, colons and periods indicate signal sequences, single fully conserved, strongly con-served and weakly concon-served residues, respectively.

Fig 2 Western blot analysis of triplatin-1 and -2 from the salivary gland of T infestans Extracts from a pair of salivary glands, recom-binant triplatin-1 and recomrecom-binant triplatin-2 were separated by 15% SDS ⁄ PAGE under reducing conditions and stained by Coo-massie brilliant blue and immunoblotted with anti-triplatin-1 serum (a-triplatin-1).

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Inhibition of platelet aggregation

by triplatin-1 and -2

To investigate the function of triplatin-1 and -2, their

effects on platelet aggregation were tested using

plate-let-rich plasma (PRP) and platelet agonists, because

they shared similarities with the known platelet

aggrega-tion inhibitor, pallidipin, as described above As shown

in Fig 3, triplatin-1 and -2 did not inhibit ADP- and

thrombin-induced platelet aggregation, but slightly

inhibited that induced by arachidonic acid and U46619,

a thromboxane A2 analog However, this weak

inhibi-tion did not titrate in a concentrainhibi-tion-dependent

man-ner, suggesting that it was an artifact In contrast, both

triplatin-1 and -2 clearly inhibited collagen-induced

aggregation in a dose-dependent manner Maximum

inhibition of 50–60% at micromolar concentrations of

triplatin-1 and -2 were recorded These results

demon-strated that triplatin-1 and -2 are inhibitors of platelet

aggregation induced by collagen

To investigate precisely the effect of triplatin-1 and

-2 on platelet aggregation caused by collagen, an

inhi-bition assay was performed using washed platelets instead of PRP In this assay, both triplatin-1 and -2 completely inhibited platelet aggregation induced by collagen (Fig 4A) Based on these results, IC50values

of triplatin-1 and -2 were calculated at approximately

60 nm and 620 nm, respectively We also examined inhibition of collagen-induced platelet aggregation using an aggregometer and PRP (Fig 4B) After sti-mulation by collagen, the characteristic peak caused by

a change of platelet shape was observed within a few minutes Triplatin-1 completely inhibited collagen-induced platelet aggregation and also attenuated the change of platelet shape

Identification of the target receptor for triplatin-1 and -2

Next, we attempted to identify triplatin-1 and -2 target molecules Collagen-induced platelet aggregation is initiated by the interaction between vWF and

GPIb-IX-V Ristocetin promotes this interaction and aggregates platelets [9–12] Therefore, we first examined the effects

Fig 3 Effect of triplatin on platelet aggregation induced by several different agonists Platelets in platelet rich plasma (PRP) (3.5–3.6 · 10 5

plateletsÆmL)1) were incubated with triplatin at 37 C for 10 min before adding collagen (2.0 lgÆmL)1), ADP (0.5 l M ), arachidonic acid (1.0 m M ) or U46619 (2.0 l M ) For stimulation by 0.1 n M thrombin, washed platelets (2.6 · 10 5

plateletsÆmL)1) were used instead of PRP Light transmittance at 600 nm was measured 10 min after stimulation, and platelet aggregation is represented as the percentage of control aggregation of platelets preincubated in the absence of triplatin Results are the mean ± SE of three experiments.

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of triplatin-1 and -2 on ristocetin-induced platelet

gation (Fig 4A) No inhibitory effect on platelet

aggre-gation induced by ristocetin was observed, indicating

that GPIb-IX-V is not a target for triplatin

Collagen-related peptide (CRP) contains the specific

GPVI recognition motif and directly activates this

receptor [26–28] Therefore, we next examined whether

triplatin-1 and -2 inhibit CRP-induced platelet

aggrega-tion Triplatin-1 and -2 did inhibit CRP-induced

plate-let aggregation in a dose-dependent manner (Fig 4A)

We also examined inhibition of collagen-induced

plate-let aggregation using an aggregometer (Fig 4B)

Trip-latin-1 almost completely inhibited CRP-induced

platelet aggregation and also attenuated the change of

platelet shape These results demonstrated that

triplat-ins inhibit platelet activation mediated by GPVI

We also assessed the effect of triplatin-1 and -2 on

platelet adhesion to immobilized soluble collagen

(Fig 5), which has been reported to be entirely

dependent on interactions between collagen and a2b1

integrin In control experiments, monoclonal antibody

against integrin a2b1, Gi9, did inhibit platelet adhesion However, triplatins did not inhibit platelet adhesion, even at a concentration of 1.0 lm

These results indicate that triplatins are specific inhibitors of collagen-induced platelet aggregation mediated by GPVI To confirm this finding, we exam-ined the effect of triplatin-1 on phosphorylation of the FcR c-chain [5,13,14] This was achieved by immuno-precipitation, because the binding of GPVI to collagen causes tyrosine phosphorylation of the FcR c-chain, which is coupled to GPVI In the absence of

triplatin-1, phosphorylated FcR c-chain of platelets stimulated

by 10 lgÆmL)1 collagen was clearly detected (Fig 6)

In contrast, in the presence of 1.0 lm triplatin-1, phos-phorylation of FcR c-chain was completely absent

Discussion

GPVI is a surface signaling receptor on platelets and has a central role in platelet activation by collagen [10] Here, we have identified a novel type of platelet

Fig 4 (A) Effect of triplatin on platelet aggregation induced by agonists of collagen receptors Platelets in PRP (3.4 · 10 5 plateletsÆmL)1) incubated with triplatin were stimulated 1.25 mgÆmL)1ristocetin Washed platelets (3.3–3.4 · 10 5 plateletsÆmL)1) incubated with triplatin-1 were stimulated with 2.0 lgÆmL)1collagen or 0.25 lgÆmL)1CRP Further methods are as in Fig 3 legend (B) Anti-aggregatory properties of triplatin on collagen- or CRP-induced platelet aggregation Washed platelets (3.0 · 10 5

plateletsÆmL)1) incubated with triplatin-1 at 37 C for

2 min were induced to aggregate by 2.0 lgÆmL)1of collagen or 0.2 lgÆmL)1of CRP After stimulation, light transmittance was monitored by aggregometer for 10 min.

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aggregation inhibitor, triplatin-1 and its isoform,

trip-latin-2, which specifically inhibit platelet aggregation

induced by collagen, especially by CRP, a specific

agonist of GPVI [26–28] Furthermore, triplatin-1

inhibited tyrosine phosphorylation of FcR c-chains

induced by collagen, the initial step in the GPVI

signa-ling cascade [13,14] These results strongly suggest that

triplatin-1 and -2 are antagonists for GPVI To the

best of our knowledge, triplatin-1 and -2 are the first

natural inhibitors for GPVI to be identified

The injured arterial wall exposes collagen to the blood and recruits platelets to the injured site In the physiological state, in which shearing has an important role, GPVI is involved in recruitment and subsequent aggregation of platelets It was reported that platelets from GPVI-deficient mice show no adhesion to colla-gen and no aggregation [9] In humans, platelets from GPVI-deficient patients can attach to collagen but nonetheless do not form aggregates These findings suggest that GPVI is crucial for thrombus formation after arterial injury [13] Feeding activities of hemato-phagous arthropods injure the blood vessels of host animals It is likely that triplatin-1 and -2 are injected into the host during T infestans blood feeding and attenuate host hemostasis at the initial phase

To date, some other inhibitors of collagen-induced platelet aggregation have been reported in the saliva

of blood-sucking arthropods Among them, pallidipin and moubatin are similar to triplatin in their inhibitory properties Like triplatin, pallidipin and moubatin inhi-bit platelet aggregation induced by collagen but not by other agonists [25] They also exert potent inhibitory effects on both platelets in plasma and washed plate-lets Furthermore, unlike other inhibitors of collagen-induced platelet aggregation, such as LAPP [19–21] and Calin [22], they do not inhibit the platelet adhe-sion to collagen mediated by a2b1integrin under static conditions [23,24] Although their mechanisms of action are not fully understood, it is possible that pal-lidipin and moubatin are also GPVI antagonists

In summary, we have identified inhibitors of colla-gen-induced platelet aggregation from the saliva of

T infestans Platelet–collagen interactions have an important role in thrombus formation, and GPVI plays a pivotal role therein Further investigations on the inhibitory mechanisms of these insect proteins might lead to development of antiplatelet agents that antagonize thrombus formation at the initial phase

Experimental procedures

Materials

Prostaglandin E1, deoxycholate, sodium orthovanadate and genenase were purchased from Biogenesis Ltd (Poole, UK), Nakarai Tesque, Inc (Kyoto, Japan), ICN Biomedi-cals, Inc (Aurora, OH, USA) and New England Biolabs, Inc (Beverly, MA, USA), respectively Apyrase, phenyl-methylsulfonyl fluoride, leupeptin and aprotinin were pur-chased from Wako Pure Chemical, Ind Ltd (Osaka, Japan) Collagen, ADP and ristocetin were purchased from Chronolog, Corp (Havertown, PA, USA) U46619, thrombin, fibrinogen and Gly-Pro-Arg-Pro peptide were

Fig 5 Effect of triplatin on platelet adhesion to collagen 3.0 · 10 5

washed platelets ⁄ well were incubated with triplatin-1, -2 or

mono-clonal antibody against integrin a2b1(Gi9) for 10 min and introduced

into wells coated with 2.0 lgÆwell)1 collagen After washing, the

adherent platelets were quantified using a protein assay The

relat-ive number of adherent platelets is presented Results are the

mean ± SE of three experiments.

Fig 6 Inhibition of the phosphorylation of FcR c-chain by triplatin.

Anti FcR c-chain immunoprecipitates were prepared from lysates of

platelets stimulated by 10 lgÆmL)1collagen (10 lgÆmL)1) in the

pres-ence or abspres-ence of 1.0 l M triplatin-1 and analyzed by anti-FcR c-chain

(aFcR c-chain) and antiphosphotyrosine (aPY) immunoblotting.

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purchased from Calbiochem (San Diego, CA) CRP was a

kind gift of H Takayama of Kyoto University

Arachido-nic acid, Nonident P-40, and other chemicals were

pur-chased from Sigma-Aldrich, Inc (St Louis, MD, USA)

Isolation and sequencing of cDNA clones

Salivary glands of T infestans were dissected from thoraces

of unfed adults, and poly A(+) RNA was isolated from 30

pairs of salivary glands using a MicroPrep mRNA isolation

kit (Amersham Pharmacia Biotech, Ltd, Amersham,

Buck-inghamshire, UK) The salivary gland cDNA library was

constructed from this isolated mRNA using the SuperScript

plasmid system (Gibco BRL Life Technologies, Inc.,

Rock-ville, MD, USA) according to the manufacturer’s

instruc-tions From this constructed cDNA library, 550 clones

were randomly selected and their DNA sequences were

determined using ABI PRISM BigDye Terminator cycle

sequencing kits (Applied Biosystems, Foster City, CA,

USA), by ABI 310 genetic analyzer (Applied Biosystems)

The cDNA sequences of triplatin-1 and -2 were deposited

in the DNA Data Bank of Japan (DDBJ) (accession

num-ber, AB 250209 and AB 250210) Sequence similarities and

signal peptide prediction of these clones were carried out

using blast (http://www.blast.genome.ad.jp/) and signal p

programs (http://www.cbs.dtu.dk/services/SignalP/),

respect-ively Sequence alignment was performed using the clustal

wprogram (http://www.clustal.genome.ad.jp/)

Production and purification of the recombinant

protein

Triplatin-1 and -2 recombinant proteins were produced in a

baculovirus-insect cell system Full-length cDNA of

tripla-tin-1 and -2 were cloned into the BamHI site of the

baculo-virus transfer vector, pAcYM1 The Sf9 cells were

cotransfected with the constructed plasmid and linearized

baculovirus DNA, AcRp23, lacZ (Becton Dickinson

Bio-sciences, San Jose, CA, USA) Recombinant proteins from

Tn5 cells infected by the recombinant baculoviruses were

secreted into the culture medium due to their original signal

peptide sequences They were purified by a combination of

cation-exchange chromatography and gel-filtration

chroma-tography Briefly, culture supernatants containing secreted

recombinant proteins were first applied to a PD-10 column

(Amersham Pharmacia Biotech) in 20 mm sodium acetate

buffer, pH 5.2 Next, the eluted samples were applied to a

MONO S column (Amersham Pharmacia Biotech)

equili-brated with 20 mm sodium acetate buffer, pH 5.2 and

eluted with a gradient from 0 to 1 m NaCl at a flow rate of

1 mLÆmin)1 The fractions containing recombinant proteins

were pooled, concentrated by Centricon 10 (Millipore

Corp., Bedford, MA, USA) and applied to a TSK G2000

SW column (Tosoh, Tokyo, Japan) equilibrated with

50 mm Tris⁄ HCl, pH 7.4, containing 150 mm NaCl Purity

of recombinant product was established by 15.0% SDS⁄ PAGE under reducing conditions Protein concentra-tion was determined with a Coomassie protein assay kit (Pierce Biotechnology, Inc., Rockford, IL, USA) using bovine c-globulin as the standard

Preparation of antibody to triplatin-1

To obtain a large amount of triplatin-1 to use as an immu-nogen, recombinant triplatin-1 was also produced as a maltose-binding protein (MBP)-fusion protein Briefly, a cDNA fragment encoding triplatin-1 without signal peptide was amplified by PCR and cloned into an expression plas-mid, pMAL-c2q (New England Biolabs) The MBP-fused triplatin was produced using this plasmid in Escherichia coli BL21, and was purified by amylose-resin affinity chroma-tography Cleavage of the recombinant protein from MBP was achieved using genenase For antibody production, rats were immunized with the MBP-free triplatin-1 emulsified in TiterMax gold (CytRx Corp., Los Angeles, CA, USA) After the first immunization, booster immunizations were done twice at intervals of 2 weeks After the final immun-ization, whole blood was taken and antisera against tripla-tin-1 were prepared

Western blot analysis

Salivary gland proteins were separated by SDS⁄ PAGE in 5–20% gradient gels and transferred to nitrocellulose mem-branes Blotted membranes were blocked in NaCl⁄ Pi con-taining 5% skimmed milk, and incubated with primary antibody against triplatin-1, and then with alkaline phos-phatase-conjugated antirabbit IgG The signal was detected using nitroblue tetrazolium

To detect the FcR c-chain in platelets, western blot analysis was performed according to Tulasne et al [29] Platelet proteins were separated by 4–20% gradient SDS⁄ PAGE, and transferred to a polyvinylidene difluoride membrane The FcR c-chain was detected with specific antisera (Upstate Biotechnology, Lake Placid, NY, USA)

in a manner similar to that described above Tyrosine phosphorylation was detected by monoclonal antibody 4G10 (Upstate Biotechnology) The signal was detected using an enhanced chemiluminescence detection system (SuperSignal West Pico Chemiluminescent Substrate, Pierce Biotechnology)

Platelet preparation

Blood was collected from healthy human volunteers by veni-puncture on acid–citrate–dextrose anticoagulant PRP was obtained by centrifugation at 110 g for 10 min Platelets were obtained by centrifugation at 1100 g for 20 min, fol-lowing incubation for 10 min with 20 ngÆmL)1prostaglandin

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E1(PGE1), and washed three times using modified Tyrode’s

buffer (5 mm Hepes buffer, pH 7.4, 134 mm NaCl, 3 mm

KCl, 0.3 mm NaH2PO4, 2 mm MgCl2, 5 mm glucose, 12 mm

NaHCO3, 1 mm EGTA, 3.5 mgÆmL)1 bovine serum

albu-min, 20 ngÆmL)1 PGE1, 20 ngÆmL)1 apyrase) Finally,

washed platelets were resuspended in modified Tyrode’s

buf-fer, substituting 2 mm CaCl2for 1 mm EGTA The number

of platelets was counted using a hematocytometer

Effect of triplatin-1 and -2 on platelet aggregation

and adhesion

Effects of triplatin-1 and -2 on platelet aggregation were

photometrically measured according to Bednar et al [30]

PRP or washed platelets were incubated with triplatin-1

and -2 for 10 min in a 96-well flat-bottom plate

(MICROTESTTM 96, Becton Dickinson Biosciences) in

50 mm Tris⁄ HCl, pH 7.4, containing 150 mm NaCl

Plate-let aggregation was initiated by addition of 2.0 lgÆmL)1

collagen, 0.5 lm ADP, 1.0 mm arachidonic acid, 0.2 lm

U46619, 0.1 nm thrombin, 1.2 mgÆmL)1 ristocetin or

0.25 lgÆmL)1 CRP as platelet activators The reaction

mixture was stirred continuously at 37C for 10 min

Platelet aggregation was monitored by light transmittance

using a microplate reader (MPR-A4i, Tosoh, Tokyo,

Japan)

Effects of triplatin-1 and -2 on platelet aggregation

induced by collagen and CRP were also analyzed using an

aggregometer (C-500, Chronolog) PRP was mixed with

triplatin-1 or -2, and platelet aggregation was started by

addition of either 2.0 lgÆmL)1 collagen or 0.2 lgÆmL)1

CRP Platelet aggregation was monitored by light

transmit-tance in the aggregometer with continuous stirring at

37C

Inhibition of platelet adhesion was examined according

to Keller et al [19] Microtiter plates (Microtiter

Poly-styrene Base Immunoassay Plates, DYNEX Technologies,

Inc., Chantilly, VA, USA) were coated with collagen

(2.0 lgÆwell)1) in 5 mm acetic acid for 1 h at room

tem-perature, followed by addition of 1% bovine serum

albu-min for 1 h at room temperature to block the nonspecific

binding of platelets to the wells After blocking, wells

were washed three times with Hepes-buffered saline,

20 mm Hepes, pH 7.4 containing 0.14 m NaCl and 2 mm

MgCl2 Washed platelets (3.0· 105

cells) and triplatin or Gi9 (Immunotech, Marseille, France) were mixed in

Tyrode’s buffer containing 2 mm CaCl2 and 100 ngÆmL)1

PGE1 and then transferred into wells After 45 min

incu-bation, wells were washed three times with

Hepes-buf-fered saline again The number of platelets adhering to

immobilized collagen was determined using Micro BCA

Protein Assay Kits (Pierce Biotechnology) The percentage

of specifically adherent platelets was calculated on the

basis of a standard curve obtained with known numbers

of platelets

Platelet lysis and immunoprecipitation

of FcR c-chains

Immunoprecipitation was performed according to Ichinohe

et al [16] and Tulasne et al [29] Washed platelets (1· 109 cells) were incubated with 1.0 lm triplatin-1 at 37C for

10 min After incubation, platelets were stimulated by

10 lgÆmL)1 collagen at 37C for 10 min and then lyzed with an equal volume of ice-cold lysis buffer, 20 mm Tris,

300 mm NaCl, 2 mm EDTA, 2% Nonident P-40, 1% deoxycholate, 0.1% SDS, 1 mm phenylmethylsulfonyl fluor-ide, 2 mm sodium orthovanadate, 10 lgÆmL)1 leupeptin and 10 lgÆmL)1 aprotinin Non-lysed cells and debris were removed by centrifugation Platelet lysate was incubated with 1 mgÆmL)1anti-FcR c-chain antiserum at 4C After overnight incubation, protein A-Sepharose beads were added to the mixture and washed three times with 10 mm Tris, 160 mm NaCl and 0.1% Tween 20 The protein bound

to beads was eluted with Laemmli buffer and applied to SDS⁄ PAGE and western blot analysis

Acknowledgements

We thank H Takayama of Kyoto University for the generous gift of CRP This study was supported by

a grant-in-aid for Scientific Research (13006374) to HI, for Scientific Research on Priority Areas (08281103) to

YC, for Scientific Research (B) (12470060) to MY, and for Exploratory Research (10877043, 11877043 and 12877042) to YC from the Ministry of Education, Sci-ence, Culture and Sports of Japan It was also suppor-ted by a grant-in-aid for Scientific Research, Research

on Health Sciences focusing on Drug Innovation (KH23306) and Young Scientists Fellowship B (16790249) to HI from the Naito Foundation, the Japan Health Sciences Foundation and JSPS, respect-ively, and a grant from the Research for the Future Program from JSPS to YC

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