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These are pathogen-derived nonenzyme proteins that exploit the ‘molecular sexual-ity’ in the activation mechanism of plasminogen and Keywords coagulation; conformation; fibrinolysis; pla

Trang 1

Small-molecule modulators of zymogen activation in the fibrinolytic and coagulation systems

Keiji Hasumi, Shingo Yamamichi and Tomotaka Harada

Department of Applied Biological Science, Tokyo Noko University, Japan

Introduction

The coagulation and fibrinolytic systems are central

to the hemostatic mechanism This mechanism is

pri-marily responsible for preventing blood leakage and

secondarily for tissue repair and wound healing

Interactions between a variety of enzymes and

nonen-zyme components account for the finely regulated

pro-cesses in the coagulation and fibrinolytic systems [1,2]

Most of the enzymes in these systems are serine

prote-ases circulating as either inactive proenzyme or

proen-zyme forms with very low activity Thus, their

activation is a prerequisite for their function, whereas

their inhibition or inactivation is also important in the

regulation and termination of the reaction Activation

of the zymogens is a consequence of a conformational

change triggered by specific proteolytic cleavage(s) of

the zymogen [3,4] The activated enzyme catalyzes the

subsequent step or upstream reaction(s) in the cascade

to amplify and⁄ or regulate the systems The reactions

in both systems operate instantly after exposure to pathophysiological stimuli Therefore, the mechanism

of their regulation is programmed in the structure of each component of the systems, and modulation of the programmed function of the component can provide a novel means of pharmacological intervention in dis-eases associated with the coagulation and fibrinolytic systems Most extensively studied examples of zymo-gen modulation are nonproteolytic conformational activations of plasminogen by streptokinase, and pro-thrombin by staphylocoagulase (and von Willebrand factor-binding protein) These are pathogen-derived nonenzyme proteins that exploit the ‘molecular sexual-ity’ in the activation mechanism of plasminogen and

Keywords

coagulation; conformation; fibrinolysis;

plasma hyaluronan-binding protein;

plasminogen; plasminogen activator;

protease; prothrombin; urokinase; zymogen

activation

Correspondence

K Hasumi, Department of Applied Biological

Science, Tokyo Noko University,

3-5-8 Saiwaicho, Fuchu-shi,

Tokyo 183-8509, Japan

Fax: +81 42 367 5708

Tel: +81 42 367 5710

E-mail: hasumi@cc.tuat.ac.jp

(Received 29 April 2010, revised 8 July

2010, accepted 19 July 2010)

doi:10.1111/j.1742-4658.2010.07783.x

The coagulation and fibrinolytic systems are central to the hemostatic mechanism, which works promptly on vascular injury and tissue damage The rapid response is generated by specific molecular interactions between components in these systems Thus, the regulation mechanism of the sys-tems is programmed in each component, as exemplified by the elegant pro-cesses in zymogen activation This review describes recently identified small molecules that modulate the activation of zymogens in the fibrinolytic and coagulation systems

Abbreviations

AH site, aminohexyl site; EGF, epidermal growth factor; Lp(a), lipoprotein(a); PA, plasminogen activator; PAN domain,

plasminogen ⁄ apple ⁄ nematode domain; PHBP, plasma hyaluronan-binding protein; scu-PA, single-chain urokinase-type plasminogen activator; SMTP, Stachybotrys microspora triprenyl phenol; tcu-PA, two-chain urokinase-type plasminogen activator; t-PA, tissue-type plasminogen activator; u-PA, urokinase-type plasminogen activator.

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prothrombin (insertion of N-terminal Ile or Val into

N-terminal binding cleft of the catalytic domain,

resulting in conformational activation of the substrate

binding site and oxyanion hole required for proteolytic

activity) [5–8]

Our laboratory has been searching for

small-mole-cule natural products that enhance the fibrinolytic

system We initially aimed at identifying a candidate

small molecule that could contribute to the treatment

of thrombotic and embolic complications As a result,

we have identified several types of compounds,

includ-ing modulators of zymogen activations Detailed

anal-yses of the action of such modulators have expanded the concept of zymogen modulation, leading to the identification of additional modulators that affect the coagulation system The active compounds and their targets are summarized in Table 1 and Fig 1 Here,

we review the identification and functional character-ization of such small-molecule modulators of zymogen activation in the fibrinolytic and coagulation systems

Plasminogen modulator

The plasminogen⁄ plasmin system The plasminogen⁄ plasmin system plays a central role

in blood clot lysis [2,9] This system is also important

in other pathophysiological events in which localized proteolysis is involved [10–12] The circulating form

of plasminogen (Glu-plasminogen) is a single-chain zymogen consisting of 791 amino acids, which form the following domain structures: a plasminogen⁄ apple⁄ nematode (PAN) domain, five kringle domains and a serine protease domain (Fig 2) [13,14] It is proteolytically activated to plasmin by plasminogen activators (PAs) through specific cleavage at Arg561– Val562 Urokinase-type and tissue-type PAs (u-PA and t-PA, respectively) are major physiological activators

Table 1 Small-molecule zymogen modulators identified in this

labo-ratory PHBP, plasma hyaluronan-binding protein; scu-PA,

single-chain urokinase-type plasminogen activator; SMTP, Stachybotrys

microspora triprenyl phenol.

Plasminogen Complestatin and chloropeptin I [43,44,52]

Staplabin and SMTPs [45–53]

scu-PA ⁄ plasminogen

reciprocal activation

Surfactins and iturins [68,69]

Glucosyldiacylglycerol [70]

Pro-PHBP Polyamines and carminic acid [104]

OH

H O

N

H

HOOC

OH

O

N H O

O

O N

O O

OH Cl

Cl

OH

HN O

OH Cl

HOOC N

H N H

O S NH

NH S

NH

S NH

O NH R

NH OH

CH 2 O

CH 2 O

CH 2 O

CH 2 O N

N

CH 2

O

CH2 O N

O N O N

O

O N

N O R O

OH HO

O

CH 3

COOH OH OH

HO

O HO

OH

OH OH

O

HO

O

HN

N NH NH NH H HN

O

O

O

O O

O

O OH

Glu

Leu

D-Leu

Leu

Val

Asp

D-Leu

NH

NH2 HN

NH N HN O

O O O

O

D-Leu

Phe

Leu

HN

NH H

O

O O

O O

S S D-Cys

D-Cys

Val

Ile

D-Leu

O

H HO

CHO CHO

O

HO OH OH

OR 2

OR 1

Complestatin

Thioplabins

Staplabin/SMTPs

Stachybotrydial

Glucosyldiacylglycerol

Surfactin C Plactin D Malformin A1 Carminic acid

HO

Fig 1 Structures of the modulators of zymogen activation R in the thioplabin structure corresponds to –CH3, –CH2CH3or –CH(CH3)2for thioplabin A, B or C, respectively R in the structure of SMTPs represents one of a variety of substituents, most of which are derived from amino acids R1and R2in the structure of glucosyldiacylglycerol correspond to the oleoyl or palmitoyl group Malformin A1, which enhances cellular fibrinolytic activity through a mechanism distinct from direct modulation of zymogen activation, is shown to compare its structure with that of plactin D.

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[2] Glu-plasminogen adopts a closed conformation

because of the intramolecular binding of Lys50 and⁄ or

Lys62 to the fifth kringle domain (K5) (Fig 3) [15,16]

The tight conformation renders Glu-plasminogen

less sensitive to activation by PAs [17,18] The

Glu-plasminogen binding to fibrin or cellular receptors

allows relaxation of Glu-plasminogen conformation,

enabling efficient activation (Fig 3) This mechanism

facilitates localized activation of plasminogen and

extracellular proteolysis [19,20] Growing evidence

sup-ports the idea that cellular plasminogen binding plays

roles in physiological processes such as macrophage

recruiting, leukocyte migration and liver regeneration

[21–24]

During the course of fibrinolysis, Lys-plasminogen

(Fig 2), a truncated form of Glu-plasminogen,

pre-dominantly with an N-terminal Lys78, appears

through autoproteolysis by the resulting plasmin

[25,26] The molecule no longer has the PAN domain

and therefore adopts a relaxed conformation [27] because of the lack of intermolecular binding between the PAN domain and K5 (Fig 3) Lys-plasminogen is highly sensitive to activation even in the absence of fibrin or cells

PAN–K5 binding is mediated via the aminohexyl (AH) site in K5 [28,29] (Fig 3) Unlike lysine-binding sites in K1, K2 and K4 of plasminogen, the AH site can bind an internal lysine residue in addition to the C-terminal lysine [30], which is a preferred ligand for the lysine-binding site in K1, K2 and K4 Thus, amin-ohexyl or lysine analogs can interfere with PAN–K5 binding and relax Glu-plasminogen conformation, ren-dering Glu-plasminogen susceptible to activation by PAs [31,32] Some proteins, as well as cell-surface plas-minogen receptors, interact with kringles and modulate plasminogen activation [33,34] It is postulated that the fibrinolytic process proceeds as follows [35]: at an ini-tial phase, the K5–fibrin interaction accumulates Glu-plasminogen on fibrin Subsequently, partially degraded fibrin, which has C-terminal lysines, plays a role in fibrinolytic propagation by serving as more effi-cient binding sites for plasminogen The high-affinity lysine-binding sites in K1 and K4 may be involved in this propagation process Thus, plasminogen binding is essential for the fibrinolytic process The kringle ligands, however, inhibit plasminogen binding to fibrin and cellular receptors and, therefore, suppress fibrino-lysis This is the basis of the antihemorrhagic action of lysine analogs such as tranexamic acid and 6-amino-hexanoic acid [36]

Competition in the binding between plasminogen and fibrin or cellular receptors can occur via physio-logic molecules Lipoprotein(a) [Lp(a)], a risk factor for coronary heart disease [37,38], is a plasma lipopro-tein related to low-density lipoprolipopro-tein In the Lp(a) molecule, apolipoprotein B-100, which is a sole protein component of low-density lipoprotein, is covalently modified with apolipoprotein(a), a protein closely related to plasminogen, consisting of multiple (11–50 repeats) K4-like domains, a K5-like domain and a pseudo-protease domain [39,40] Lp(a) can compete with plasminogen for binding to fibrin or cell-surface receptors and attenuate localized plasminogen activa-tion [41] and conversion of Glu-plasminogen to Lys-plasminogen [42] These findings suggest a possible link between thrombosis and atherosclerosis

Our laboratory has screened up to 10 000 microbial cultures for their ability to enhance Glu-plasminogen binding to fibrin or culture cells This attempt is based

on the hypothesis that relieving the plasminogen bind-ing competition might enhance fibrinolytic activity The active compounds identified include complestatin

Gla K1

P

R I

T 285 321 320

K

E K I P

S 1

A 1

F 1

F 1

S 1

159 158

K4 K1 K2 K3 K5 P

E 1

K 78

K 78

K4 K1 K2 K3 K5 P

R

K4 K1 K2 K3 K5 V P

562

E1 E2 E3 K P

R

E1 E2 E3 K I P

291 290

PAN

Prothrombin

α-Thrombin

Glu-plasminogen

Pro-PHBP

PHBP

Lys-plasminogen

Plasmin

scu-PA

tcu-PA

561

Fig 2 Structures of key zymogens and their active forms Each

molecule is shown schematically with each domain in a colored

circle The disulfide bond that connects the A- and B-chains of the

mature protease is shown in green Red lines in the PHBP

molecule represent the N-terminal region (NTR) PAN, PAN domain;

K, kringle domain; P, protease domain; Gla, c-carboxyglutamic acid

domain; E, EGF domain.

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[43] and its isomer chloropeptin I [44], staplabin [45]

and its congener Stachybotrys microspora triprenyl

phenols (SMTPs) [46–53], thioplabins [54] and

stachyb-otrydial [55]

Complestatin and chloropeptin I

Tachikawa et al [43] isolated complestatin, a

chlorine-containing peptide metabolite from Streptomyces sp.,

as an active principle that enhanced Glu-plasminogen

binding to cultured U937 monocytoid cells

Complest-atin enhances the binding by several fold at 1–10 lm

The enhancement is observed in either the absence or

presence of Lp(a) The compound is also effective in

elevating Glu-plasminogen–fibrin binding The actions

of complestatin are canceled by a lysine analog Thus,

the target of complestatin is Glu-plasminogen, and the

agent promotes its binding to fibrin and cells via the

AH site or the lysine-binding sites However, the initial

characterization does not clarify the exact mechanism

of the complestatin actions The current understanding

is that the action of complestatin modulates

Glu-plas-minogen conformation [52], but verification of this has

awaited the characterization of staplabin and SMTPs

However, the concept that small molecule-mediated

augmentation of plasminogen binding results in

increased plasmin formation on cell surfaces has been

confirmed by experiments using complestatin [43]

Chloropeptin I, an isomer of complestatin, has a

similar but slightly different effect on plasminogen

binding compared with complestatin [44]

Chloropep-tin I is 3–10 times more active than complestaChloropep-tin in

enhancing cellular binding of Glu-plasminogen,

cell-surface plasmin formation, and whole-blood

fibrinolysis assessed by thromboelastography, although the agent is less active in promoting fibrin binding of Glu-plasminogen Although the structural difference between complestatin and chloropeptin I is only at the position of the C–C bond that connects the indole ring

of the tryptophan residue and the aromatic ring of the 3,4-dihydroxyphenylglycine residue, a large difference

in conformation between the two compounds is evident from the nuclear Overhauser effect in NMR spectroscopy It is speculated that this difference may account for the distinct activities of the two compounds [44]

Staplabin and SMTP Shinohara et al [45] discovered a novel triprenyl phe-nol compound, named staplabin, from a culture of the fungus Stachybotrys microspora, as an active principle that enhanced Glu-plasminogen binding to fibrin Later, several new staplabin congeners, SMTPs, were isolated by Kohyama et al [46], Hasumi et al [48,53], and Hu et al [49,51] These are named after Stachybot-rys microspora triprenyl phenol The staplabin⁄ SMTP molecule consists of a tricyclic c-lactam moiety, an iso-prene side chain and an N-linked side chain (Fig 1) Most of the congeners differ in the N-linked side chain moiety, which is essential for their activity The N-linked side chain can be derived from an amine present in the culture medium, and this finding enabled selective, efficient production of SMTP congeners through an amine-feeding cultivation of S microspora [50,51,53]

Staplabin enhances Glu-plasminogen binding to both fibrin and cultured U937 cells [45] These

K4 K2

K5 P

Fibrin or cellular receptor

PA

K 78

K 78

K4

K1

P

R 561

V 562

Glu-plasminogen

(Closed conformation)

Plasmin

(Open conformation)

K4 K2

K5

P K1

Lys-plasminogen

(Open conformation)

E 1

E 1

P K3 K2 K1

K5 K4 K PAN

50

PAN

D55 D57 W62

W64

F36

Y72

I35 L71 H33 H31

K5 structure

K3

K2 K3 K5

K1

K3

Fig 3 A model of the conformational regulation of plasminogen activation The plasminogen and plasmin molecules are shown as in Fig 2 The schematic conformation shown is speculative, because detailed experimental data are not yet available Key disulfide bonds are shown

in green The molecular structure K5 is shown in the right-hand box The electrostatic surface image, in which areas of neutral, negativeand positive potential are depicted in white, red and blue, respectively, was constructed using the coordinate deposited in the RCSB Protein Data Bank with the code number 2KNF The labeled amino acids are those implicated in the binding of the lysine analog tranexamic acid [29].

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bindings are mediated by the lysine-binding site or the

AH site, because a lysine analog inhibits the bindings

These activities are quite similar to those of

complesta-tin and chloropepcomplesta-tin I Takayasu et al [47] show that

staplabin promotes PA-dependent Glu-plasminogen

activation The two staplabin activities, the elevation

of Glu-plasminogen-fibrin binding and the promotion

of Glu-plasminogen activation, are observed at the

same range of staplabin concentrations Thus, a

com-mon mechanism may govern the two effects The fact

that the activation of Glu-plasminogen is a

conforma-tionally regulated process is the key to understanding

this mechanism The effect of staplabin on the

activa-tion of Lys-plasminogen, which adopts an open

con-formation, is less prominent than its effect on

Glu-plasminogen Similarly, smaller effects of staplabin on

Glu-plasminogen activation are observed in the

pres-ence of the lysine analog 6-aminohexanoic acid or

fibrinogen fragments, both of which relax

Glu-plasmin-ogen conformation The molecular elution time of

both Glu-plasminogen and Lys-plasminogen is slightly

but significantly shortened in the presence of staplabin

These results support the idea that the staplabin effects

are related to the conformational status of

plasmino-gen, and Takayasu et al [47] have concluded that

staplabin modulates plasminogen conformation,

rendering the molecule susceptible to proteolytic

acti-vation and to binding to cells and fibrin The reason

why the effects of staplabin on Glu-plasminogen is

lar-ger than its effect on Lys-plasminogen can be

explained by the fact that the impact of the

conforma-tional effect depends on the initial conformaconforma-tional

status of plasminogen With respect to the

conforma-tional modulation that leads to an elevated

Glu-plasminogen activation, the staplabin effect is similar

to that of lysine analogs, whereas the effects of each

compound on plasminogen binding are quite different

This implies that staplabin acts as a plasminogen

modulator that works through a mechanism distinct

from the lysine-binding site (or AH site) occupancy

Staplabin congener SMTPs may act on plasminogen

activation and binding similarly to staplabin, whereas

some congeners, such as SMTP-7 and -8, are far more

potent than staplabin [49] The action of

stapla-bin⁄ SMTP is shown schematically in Fig 4

Pharma-cological evaluations of SMTP-7 suggest that the

compound is a promising candidate drug for treating

thrombotic and embolic complications Detailed

inves-tigations are now under way

Plasmin formation in the presence of SMTP is

tran-sient in an incubation of Glu-plasminogen with u-PA

[52] A decrease in plasmin activity follows a rapid

increase in plasmin formation This is because of

auto-proteolytic degradations of the catalytic domain of the plasmin molecule Ohyama et al speculate that the conformational change brought about by SMTP affects susceptibility to autoproteolytic cleavage 6-Aminohexa-noic acid does not lead to autoproteolysis, but enhances plasminogen activation Thus, the difference between conformational modulation by SMTP and that by the lysine analog is also evident from these results Similar promotion of plasmin autoproteolysis is observed with complestatin [52] This effect is obtained with a concen-tration range identical to that effective in enhancing Glu-plasminogen binding, suggesting complestatin’s action as a plasminogen modulator As expected, com-plestatin-mediated enhancement of Glu-plasminogen activation has been confirmed

Thioplabins Ohyama et al [54] identified thioplabins (or antibiotic A10255) (Fig 1), a family of thiopeptide metabolites from Streptomyces sp., as modulators of plasminogen binding Thioplabin B enhances the binding of both Glu-plasminogen and Lys-plasminogen to fibrin It also promotes PA-dependent activation of Glu- and Lys-plasminogen Like staplabin, the effect of thiopla-bin B is smaller on conformationally relaxed Lys-plas-minogen Thioplabin B alters patterns of proteolytic degradation of Glu- and Lys-plasminogen upon

E 1

K4

E 1

Fibrin or cellular receptor

Glu-plasminogen

(Conformational change)

Modulator

PAN

P

K2 K1

K5 K4 K3

K 50

K2 K3

K4

K1

P K5 R 561

V 562

Plasmin

PA

K2 K3

E 1

PAN

P

K3 K2 K1

K5

50

K5

Fig 4 A model of the action of the plasminogen modulator stapla-bin ⁄ SMTP Staplabin and SMTP alter plasminogen conformation and enhance both PA-dependent plasminogen activation and bind-ing to fibrin or cellular receptors Although these compounds can also modulate the functions of Lys-plasminogen, the magnitude of the effects is small, possibly because Lys-plasminogen adopts a more relaxed conformation compared with Glu-plasminogen The schematic model shows only the modulation of Glu-plasminogen function.

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incubation with elastase The agent also increases

auto-proteolytic degradation of the plasmin catalytic

domain [52] These features conform to the concept of

the nonlysine-analog plasminogen modulator

estab-lished by staplabin⁄ SMTP Thioplabin analogs that

lack the terminal carboxyl group are inactive in

plasminogen modulation [54]

Stachybotrydial

Stachybotrydial (Fig 1) is a tripreny phenol metabolite

from Stachybotrys sp., structurally distinct from

staple-bin⁄ SMTPs Sasaoka et al [55] show that

stachybotry-dial has a specific effect on Glu-plasminogen It

enhances the activation and fibrin binding of

Glu-plas-minogen, but not Lys-plasminogen Unlike the

modu-lation of plasminogen function by other small

molecules described above, the action of

stachybotry-dial involves covalent modification of

Glu-plasmino-gen Because covalent stachybotrydial modification is

observed even with Lys-plasminogen, the selective

effects on Glu-plasminogen are related to its

confor-mational status Thus, stachbotrydial represents

another class of plasminogen modulators in addition

to complestatin⁄ chloropeptin I, staplabin ⁄ SMTP and

thiplabins, which reversibly modulate the function of

Glu- and Lys-plasminogen

Modulator of the reciprocal activation

of single-chain u-PA and plasminogen

Reciprocal activation of single-chain u-PA and

plasminogen

Of the two major physiological plasminogen activators,

t-PA is postulated to play a role in fibrin dissolution in

the circulation, whereas u-PA is involved in pericellular

proteolysis [2] t-PA has a significant affinity for fibrin

and exhibits activity more than two orders of magnitude

higher in the presence of fibrin through the formation of

a cyclic ternary complex with plasminogen and fibrin

[56,57] u-PA, which consists of an epidermal growth

fac-tor (EGF) domain, a kringle domain (which does not

contain a lysine-binding site) and a protease domain

(Fig 2), has little affinity to fibrin and utilizes a distinct

mechanism to regulate localized proteolysis u-PA is

syn-thesized as a single-chain zymogen (scu-PA), and binds

to the cell-surface receptor u-PAR via its EGF domain

[58,59] in an autocline manner to facilitate the activation

of cell-bound plasminogen for pericellular proteolysis

involved in a variety of conditions including tissue

remodeling, macrophage function, ovulation and tumor

invasion [60,61] scu-PA is specifically cleaved at Lys158–

Ile159 by plasmin, affording a two-chain derivative (Fig 2) that has a full protease activity [62] Thus, the reciprocal activation of scu-PA and plasminogen constitutes a mechanism of localized initiation and propagation of pericellular proteolysis [63–66] and fibri-nolysis on platelets [67] The mechanism of the initiation

of the reaction (how the two zymogens activate each other in the initial phase), however, remains to be fully elucidated

A screen of natural sources, including microbial cul-tures and plant extracts, for a modulator of the recipro-cal activation system has led to the identification of surfactins [68], iturins Cs [69] and glucosyldiacylglycerol [70]

Surfactins and iturins Surfactin C (Fig 1), a cyclic heptapeptide with a fatty acid ester in the cyclic structure, is a metabolite from Bacillussp Kikuchi and Hasumi [68] show that surfac-tin C modulates the reciprocal activation of Glu-plasminogen and scu-PA Upon incubation with Glu-plasminogen and scu-PA, the spontaneous activa-tion of both Glu-plasminogen and scu-PA proceeds slowly Surfactin C markedly enhances the concomi-tant formation of tcu-PA and plasmin The surfactin C action involves modulation of Glu-plasminogen activa-tion through relaxing the conformaactiva-tion of the protein Surfactin C increases the intrinsic fluorescence of Glu-plasminogen, shortens molecular elution time in size-exclusion chromatography, and enhances fibrin-binding and activation of Glu-plasminogen catalyzed

by tcu-PA or t-PA [68] Thus, surfactin C can be a plasminogen modulator, but the mechanism by which the agent promotes the initiation of the reciprocal acti-vation is not fully understood A possible explanation would be that the modulation of Glu-plasminogen con-formation allows cleavage by scu-PA, which has very low intrinsic activity toward native Glu-plasminogen (< 0.4% of tcu-PA [71]) Surfactin C, in combination with scu-PA, significantly enhances thrombolysis in a rat pulmonary embolism model [68]

Surfactin C belongs to a large family of lipopeptides that includes surfactins (heptapeptides consisting of two acidic and five aliphatic amino acids), iturin As (heptapeptide consisting of six polar amino acids and

a proline) and iturin Cs (heptapeptide consisting of five polar and an acidic amino acids as well as a proline) All the surfactins and iturin As tested are effective in enhancing the reciprocal activation and tcu-PA-catalyzed Glu-plasminogen activation, whereas iturin Cs, which contain no carboxyl group, are inac-tive [69]

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Wu et al [70] identified glucosyldiacylglycerol (Fig 1),

a cellular constituent of the seaweed Sargassum

fulvel-lum, as a stimulator of the reciprocal activation of

scu-PA and Glu-plasminogen The apparent action of

glucosyldiacylglycerol is similar to that of surfactin C

in that it leads to the mutual activation of scu-PA and

Glu-plasminogen Unlike surfactin C, however,

gluco-syldiacylglycerol minimally affects Glu-plasminogen

activation catalyzed by tcu-PA and t-PA Thus, the

agent likely represents a different class of zymogen

modulator than the plasminogen modulators

Gluco-syldiacylglycerol markedly enhances scu-PA-mediated

Glu-plasminogen activation in the absence of the

con-version of scu-PA to tcu-PA Upon incubation with

glucosyldiacylglycerol, the intrinsic fluorescence of

scu-PA, but not tcu-PA or Glu-plasminogen, increases

significantly Thus, glucosyldiacylglycerol may act on

scu-PA to draw intrinsic PA activity in the zymogen

The agent enhances fibrin dissolution mediated by

scu-PA and Glu-plasminogen

Modulator of the activation of

prothrombin

Prothrombin activation

The formation of thrombin from its zymogen

prothrom-bin is the central event in the coagulation cascade In

addition to the conversion of fibrinogen to fibrin,

thrombin orchestrates the coagulation and fibrinolytic

processes through activation of factors V, VIII, XI and

XIII [1], as well as protein C [72] and

thrombin-activat-able fibrinolysis inhibitor [73] after binding to

thrombo-modulin In addition, thrombin triggers a variety of

cellular responses by binding to and specifically cleaving

the extracellular domain of the family of

G-protein-cou-pled receptors, protease-activated receptors [74]

Pro-thrombin, a 579-amino-acid glycoprotein, consists of a

c-carboxyglutamic acid domain, two kringle domains

and a protease domain (Fig 2) [75] Prothrombin

acti-vation is due to proteolytic cleavage at Arg320–Ile321,

followed by cleavage at Arg271–Thr272 [76–78] An

additional cleavage at Arg284–Thr285 by thrombin

itself affords mature a-thrombin At the site of vascular

injury, prothrombin is rapidly activated to thrombin by

the coagulation factor Xa which is Ca2+-dependently

assembled with factor Va on acidic phospholipid

mem-branes of damaged vascular endothelium or activated

platelet aggregates [76,79–82] Activation of

prothrom-bin by the complex (prothromprothrom-binase complex) is

more than 105 times faster than that by free Xa [83]

Therefore, physiological coagulation is essentially cata-lyzed by the prothrombinase complex

Dual modulation of prothrombin activation by plactin

Inoue et al [84] discovered a family of novel cyclic pentapeptides after screening microbial cultures for agents that enhanced cellular fibrinolytic activity in an incubation of U937 cells with plasma The cyclopenta-peptides, designated plactins, consist of an aromatic (Phe or Tyr), a basic (d-Arg) and three bulky aliphatic amino acids (d-Val, Leu and d-Leu or d-allo-Ile) (see Fig 1 for the structure of plactin D) The structure– activity relationships of 50 synthetic plactins demon-strate that a sterically restricted arrangement of four hydrophobic amino acids and a basic amino acid is essential for their activity [85] Plactin increases U937 cell-mediated fibrin degradation, which depends on the presence of plasma The profibrinolytic action of one

of the promising compounds, plactin D, has been demonstrated in animal experiments [85]

The action of plactin involves an increase in cellular u-PA activity [85] In this mechanism, the presence of plasma is an absolute requirement The plasma depen-dency is characterized in detail by Harada et al [86], because plasminogen alone cannot substitute for plasma, and the presence of a cofactor for the plactin action is suggested On cultured U937 cells, most of the u-PA molecules exist in the zymogen form,

scu-PA Upon treatment with plactin in the presence of plasma, scu-PA converts to the two-chain form Thus, plactin, in combination with a plasma cofactor, aids proteolytic activation of cellular scu-PA It is interest-ing that malformin A1 (Fig 1), which belongs to another family of cyclopentapeptides, has plasma-dependent activity to promote cellular fibrinolytic activity [87] Although the structural features of mal-formin partially resemble that of plactin, the mecha-nisms involved in their actions are quite different The malformin action does not involve the increase in cellular u-PA activity [87]

Using plactin-affinity gels, Harada et al [86] identi-fied prothrombin as a candidate for a cofactor from plasma The actions of plactin and prothrombin that lead to the activation of scu-PA are explained as follows: (a) plactin binds to prothrombin, alters its conformational status and therefore modulates prothrombin activation by factor Xa; (b) the conse-quence of the modulation under the conditions of the assay for cellular fibrinolytic activity is the promotion

of prothrombin activation; (c) the resulting thrombin can cleave scu-PA at Arg156–Phe157 (two residues

Trang 8

proximal to the activation cleavage site, Lys158–

Ile159) to form an inactive two-chain u-PA species;

and (d) the tcu-PA derivative, in turn, is processed

to active tcu-PA by dipeptidyl peptidase I-like activity

of U937 cells, possibly through the removal of

Phe157–Lys158 from the newly formed N-terminus

(Fig 5)

The plactin-modulation of prothrombin activation

leads to different outcomes depending on the form of

the catalyst factor Xa [86] Plactin inhibits

prothrom-bin activation by factor Xa associated with acidic

phospholipid membranes, especially by the

prothrom-binase complex, which accounts for the physiological

coagulation reaction By contrast, plactin enhances

prothrombin activation by membrane-free Xa,

result-ing in increased formation of a-thrombin The

activa-tion of prothrombin is conformaactiva-tionally regulated

The specificity of prothrombinase for prothrombin is

mediated by exosites, which are physically separated

from the catalytic site It has been postulated that

sub-strate recognition by prothrombinase involves a

two-step mechanism with an initial docking of prothrombin

to the exosites, followed by a conformational change

to engage the Xa catalytic site [88] The

plactin-medi-ated dual modulation of prothrombin activation may

be related to the alteration of prothrombin

conforma-tion induced by the agent

Modulator of the activation of plasma

hyaluronan-binding protein

Plasma hyaluronan-binding protein activation

Plasma hyaluronan-binding protein (PHBP;

alterna-tively designated factor VII activating protease) is a

protease that is implicated in both the coagulation and

fibrinolytic systems, because the enzyme catalyzes the activation of factor VII and scu-PA [89,90] It is sug-gested that PHBP plays a role in the regulation of inflammation [91], vascular function [92], neointima formation [93], liver fibrosis [94,95] and atherosclerosis [92,96] PHBP exists in plasma as a single-chain zymo-gen form (pro-PHBP) at a concentration of 170 nm Pro-PHBP consists of 537 amino acids which form the following domains: an N-terminal region, three EGF domains, a kringle domain and a protease domain (Fig 2) [97] The pro-PHBP activation occurs via cleavage at Arg290–Ile291 No physiologically relevant protease that can activate pro-PHBP has been found Alternatively, pro-PHBP can be activated autoproteo-lytically Negatively charged molecules such as heparin and RNA accelerate pro-PHBP autoactivation [98– 101], possibly by serving as a scaffold for the accumu-lation of pro-PHBP, whereas pro-PHBP activation is observed only after hepatic injury, partial hepatectomy [102] or inflammation [103] Thus, pro-PHBP activa-tion may be a highly regulated process and a particular mechanism should be involved in pathophysiological pro-PHBP activation

Polyamines: promotion of pro-PHBP autoactivation complex formation Yamamichi et al [104] searched for inflammation-asso-ciated factors that promote pro-PHBP activation and identified polyamines as potential candidates The polyamines, for example, putrescine, spermidine and spermine, are cationic small molecules that accumulate

in cells undergoing rapid growth and play a role in the regulation of proliferation, differentiation and pro-grammed cell death [105,106] Spermidine markedly enhances intermolecular association of pro-PHBP to form the ‘autoactivation complex’ [104] The impor-tance of the complex formation is supported by the result that a ‘pro-PHBP decoy’, with its active site Ser486 replaced by Ala (S486A), efficiently inhibits the autoactivation The experiments aided by a series of domain-deletion mutants prepared based on the S486A mutant show that: (a) the mutant lacking the third EGF domain (DE3) cannot form the autoactivation complex; (b) heparin, which binds the third EGF domain, inhibits the complex formation; (c) N-terminal region binds to the mutant lacking N-terminal region (DN) and this binding is inhibited by heparin; and (d) spermidine binds to pro-PHBP but not to the DN mutant Thus, the N-terminal region participates in the formation of the pro-PHBP autoactivation complex, and this function is regulated by spermidine (Fig 6) [104]

R

S 1

156

P

S 1

scu-PA (inactive) Thrombin-cleaved

tcu-PA derivative (inactive)

tcu-PA (active)

α-Thrombin

F

Plactin

Prothrombin

Xa

DPP-I-like peptidase

P

R

156

R

P

156

157

I

Fig 5 Prothrombin-mediated pathway to cellular scu-PA activation

promoted by plactin The scu-PA molecule is shown schematically

as in Fig 2 The amino acids involved in proteolytic cleavages are

given in white circles DPP-I, dipeptidyl peptidase I.

Trang 9

Carminic acid: specific inhibition of

polyamine-mediated pro-PHBP autoactivation

On the basis of the specific effects of polyamines,

Nishimura et al screened natural sources for an

inhi-bitor of spermidine-induced pro-PHBP activation [107]

and identified several small molecules including

carmi-nic acid [104], an anthraquinone derived from the

cochineal insect Carminic acid inhibits

spermidine-promoted pro-PHBP autoactivation selectively, and

does not affect the autoactivation in the absence of

spermidine or that induced by negatively charged

mol-ecules such as heparin or RNA It also has no effect

on the catalytic activity of the active form of PHBP

This specific effect is due to the inhibition of

autoacti-vation complex formation (Fig 6) Carminic acid may

modulate the polyamine-dependent N-terminal region

function, because the agent inhibits binding between

the N-terminal region and DN only in combination

with spermidine [104] The features of carminic acid,

as well as of polyamines, conform to the idea of the

zymogen modulator

Conclusions and perspectives

The activation of zymogens, particularly those in the

coagulation and fibrinolytic systems, are regulated by

fine mechanisms programmed in their molecules The

small molecules described here act by utilizing or

mod-ulating such embedded mechanisms and do not affect

the catalytic activity of the mature enzymes These

fea-tures discriminate zymogen modulators from inhibitors

or activators that simply act on mature enzymes

Zymogen activation is an allosteric process, and the

zymogen modulators are allosteric effectors acting

dur-ing zymogen activation Selective inhibitors or

antago-nists⁄ agonists have been used as a pharmacologically

powerful means to treat a variety of diseases Zymogen

modulators will contribute to the development of novel

classes of drugs, as their actions are an ideal

on-demand system, which operates where and when the

physiological system is prompted to work, depending

on the physiological supply of the enzyme that acti-vates the zymogen

Acknowledgements

We would like to thank the laboratory staff for their contribution to the studies of zymogen activation mod-ulators, Eriko Suzuki for critical reading of the manu-script and Takashi Tonozuka for construction of the image of kringle 5

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