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Studies with b- and c-secretase inhibitors, as well as with the metalloproteinase inhibitor GM6001, revealed an inhibition of neuregulin-1 processing in human astroglioma cell line U373;

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Christian Freese1,*, Alistair N Garratt2, Falk Fahrenholz1and Kristina Endres1

1 Institute of Biochemistry, Johannes Gutenberg-University, Mainz, Germany

2 Department of Neurosciences, Max-Delbru¨ck-Centre, Berlin, Germany

Neuregulin-1 (NRG-1) belongs to a family of growth

factors that transduce cellular signals by binding to

ErbB receptors [1,2] At least sixteen different gene

products of NRG-1 have been identified [3,4], which

display a wide range of functions in the developing as

well as in the adult organism Besides organs such as

the heart [5,6] or breasts [7], certain isoforms of

NRG-1 mediate important properties in the central

and peripheral nervous system: synapse formation [8]

and transmission [9], expression of neurotransmitter

receptors [10–12] and synaptic plasticity [13]

Addi-tionally, general features of neurones or Schwann

cells, such as proliferation, differentiation, migratory processes and regeneration, depend on NRG-1 activity [14–17]

Although some of these functions are restricted to the developing embryonic brain, expression of NRG-1

or at least some of its isoforms [18,19] and the ErbB receptors [13,17,20,21] persists throughout the adult rodent and human nervous system Within hippo-campal synapses of adult mice, for example, NRG-1b

is implicated in activity dependent remodulation by reversing long-term potentiation [22] Moreover, it induces neurite extension and arborization of primary

Keywords

Alzheimer; ErbB; metalloproteinase;

myelination; shedding

Correspondence

K Endres, Institute of Biochemistry,

Johannes Gutenberg-University,

Johann-Joachim-Becherweg 30,

55128 Mainz, Germany

Fax: +49 6131 3925348

Tel: +49 6131 3926182

E-mail: endres@uni-mainz.de

*Present address

Institute of Pathology, Johannes

Gutenberg-University, Mainz, Germany

(Received 28 August 2008, revised 22

December 2008, accepted 6 January 2009)

doi:10.1111/j.1742-4658.2009.06889.x

Although ADAM10 is a major a-secretase involved in non-amyloidogenic processing of the amyloid precursor protein, several additional substrates have been identified, most of them in vitro Thus, therapeutical approaches for the prevention of Alzheimer’s disease by upregulation of this metalloproteinase may have severe side effects In the present study,

we examined whether the ErbB receptor ligand neuregulin-1, which is essential for myelination and other important neuronal functions, is cleaved by ADAM10 Studies with b- and c-secretase inhibitors, as well

as with the metalloproteinase inhibitor GM6001, revealed an inhibition of neuregulin-1 processing in human astroglioma cell line U373; however, specific RNA interference-induced knockdown of ADAM10 remained without effect In vivo investigations of mice overexpressing either ADAM10 or dominant negative ADAM10 showed unaltered cleavage of neuregulin-1 compared to wild-type animals As a consequence, the mye-lin sheath thickness of peripheral nerves was unaffected in mice with altered ADAM10 activity Thus, although the b-secretase BACE-1 acts as

a neuregulin-1 sheddase, ADAM10 does not lead to altered neuregulin-1 processing either in cell culture or in vivo Adverse reactions of an ADAM10-based therapy of Alzheimer’s disease due to neuregulin-1 cleav-age are therefore unlikely

Abbreviations

APLP, amyloid precursor-like protein; APP, amyloid precursor protein; APPs, soluble APP fragment; DAPT,

N-[N-(3,5-difluorophenacetyl)-L -alanyl]-S-phenylglycine t-butyl ester; NRG-1, neuregulin-1; RNAi, RNA interference.

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cultures derived from adult murine hippocampi [21].

There is substantial genetic evidence that single

nucleo-tide polymorphisms of NRG-1 are associated with the

pathogenesis of schizophrenia [23–25] In addition,

NRG-1 has been found to be involved in the

patho-genesis of other diseases such as multiple sclerosis

[26,27] or breast cancer [7]

How proteins derived from the gene for NRG-1

ful-fil their different functions exactly remains elusive:

iso-forms of type I and III exist as transmembrane iso-forms

or can be proteolytically processed [8,28–30] to release

soluble fragments It is not known in detail whether

the transmembrane protein or its proteolytic products

are mainly responsible for the different functions

Because recombinant soluble NRG-1 often is sufficient

to induce morphological or biochemical phenotypes

[21,31] and shedding of NRG-1 is activity dependent,

as shown for electrically stimulated neurones [8], an

important role of the cleavage fragments is implicated

The proteinases involved in NRG-1 proteolysis have

been partly characterized: cleavage by the amyloid

precursor protein (APP)-processing c-secretase [32,33]

and, more recently, b-secretase BACE-1 [29,34] was

analyzed both in vitro as well as in vivo Additional

data have also been reported with respect to

metallo-proteinase-derived proteolysis of NRG-1 isoforms

For example, ADAM19 was shown to participate in

NRG-1-b shedding, whereas NRG-1-a2 was not

affected by coexpression of this enzyme [35] Cleavage

of the a2 isoform of NRG-1, on the other hand, was

impaired in fibroblasts with catalytically inactive

ADAM17 [30]

b- and c-secretase are responsible for processing of

the Alzheimer associated APP and its paralogues

amy-loid precursor-like protein (APLP) 1 and APLP2 [36]

Furthermore, the distribution of NRG-1 and the

local-ization of its receptor ErbB4 have been found to be

altered in Alzheimer’s disease patients [19,37] and a

mouse model of the disease [19] ADAM10 was found

to act as a-secretase in vitro and in cultured cells

[38,39] It competes with BACE-1 for the substrate

APP and is able to prevent the formation of Ab

pla-ques in a mouse model of the disease [40] Moreover,

ADAM10 restores long-term potentiation and

increases cognitive function in transgenic mice [40,41]

and enhances cortical synaptogenesis [42] Due to the

overlap of substrate specificity of BACE-1 and

ADAM10 with respect to substrates such as APP or

the APLPs and partial phenotypic overlap of

ADAM10 and NRG-1 knockout mice [43–45], it was

considered important to investigate the possible role of

ADAM10 in NRG-1 processing in cells and in the

living animal

Results

Identification of NRG-1 isoforms expressed in the human astroglioma cell line U373

The expression and processing of NRG-1 was described previously in different astroglioma cell lines [31] Therefore, we chose the human astroglioma cell line U373 to examine the relevance of ADAM10 for NRG-1 shedding The investigated cell line stably overexpresses the human neuron specific APP isoform

695 to provide an appropriate control substrate for a- as well as b- and c-secretases [39,46]

Recently, sixteen different isoforms of NRG-1 gen-erated by alternative promoter usage, transcription initiation sites or splicing [4,47,48] have been described, and a wide variety of these isoforms are found in brain-derived cell types [49–51] To charac-terize the isoforms present in the U373 cell line, we performed RT-PCR with domain specific primers [52,53] Type I as well as type III specific PCR prod-ucts (schematically shown in Fig 1A: immunoglobu-lin-like domain and glycosylation site or cysteine rich domain sequences) were produced, whereas those characteristic of the type II Kringle domain coding region were not detectable (Fig 1B) Both a- as well

as b-type indicating PCR products were generated

We amplified the juxtamembrane region coding sequence with primers independent of a- or b-type (primers jD_for and TM_rev; Table 1) and subcloned the resulting DNA fragments into pUC19 Sequencing analysis revealed that seven out of eight clones were the a2-type, whereas only one was identified as b2 (for sequences, see Fig 1B; NM_013964 and NM_13957) Hence, the predominant NRG-1 isoform present in U373 cells is the a2-type with respect to the juxtamembrane region Because ADAMs such as ADAM10 cleave their substrates in close proximity to the membrane, knowledge of this region of the puta-tive substrate NRG-1 in the investigated cell line was mandatory

On the protein level, the NRG-1 antibody against the C-terminal domain detected a prominent band of approximately 90 kDA in the lysate of U373 cells (Fig 1C) This is consistent with full length NRG-1 in its glycosylated state [31] for a panel of glioma cells Protein bands with a higher molecular weight might indicate the immature proform and the band with a reduced molecular weight might represent an incom-pletely glycosylated intermediate Additionally, between 40 and 50 kDa, two C-terminal fragments were detectable After serum free incubation of cells for 4 h, a band of approximately 60 kDa (N-terminal

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fragment) was detected in cell supernatants using the

pan-NRG-1 antibody against the ectodomain, which

recognizes a- as well as b-isoforms (Fig 1C) This

pro-tein reveals a slightly lower molecular weight

com-pared to the results obtained by Ritch et al [31] where

secreted NRG-1 had a molecular mass of 70 kDa

Because at least two Asn residues and 11 Thr⁄ Ser

resi-dues were identified as potential sites for N- or

O-gly-cosylation of NRG-1 [54], the deviation in the size of

the soluble protein fragment may depend on different glycosylation patterns in the investigated cell lines In mouse brain membranes, a panel of proteins in the approximate range of 160–70 kDa was observed (Fig 1C), which corresponds to NRG-1 species described for mouse brain as well as human brain material [19] Similar to cell supernatants, the soluble fraction of mouse brain contained a secreted form of NRG-1 of 55–60 kDa

Fig 1 Isoforms of NRG-1 expressed in the human astroglioma cell line U373 and mouse brain (A) In general, three major types of NRG-1 are generated, which all share an EGF-like domain; further variation is achieved through differences in the sequences of the C-terminal part of the EGF domain (a or b) isoforms, and the juxtamembrane region (e.g a2 or b1 isoforms) and other domains such

as the type II specific Kringle or the type III specific cysteine-rich domain (B) To identify mRNA species of NRG-1 present in the human astroglioma cell line U373, RT-PCR was performed A sample lacking RNA was used as a no template control (NT) and a GAPDH sequence was amplified for the reaction control (C) NRG-1 protein expression in U373 cells and mouse brain was analyzed using the antibody against the C-terminus or against the extracellular domain Cell lysate or the membrane fraction from mouse brain was subjected to 4–12% NuPAGE and cell supernatants (medium) or soluble proteins from mouse brain were subjected to 8% SDS ⁄ PAGE NRG-1 protein species (FL, full length; NTF, N-terminal fragment; CTF, C-terminal fragment) were visualized after transfer onto poly(vinylidene difluoride) membrane.

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Table 1 Primer sequences used for NRG-1 isoform analysis.

Length of amplificate (bp)

NRG-TM_rev

TGAAAGACCTTTCAAACCCCTC GTTTTGCAGTAGGCCACCAC

Approximately 200 (depending on isoform) Immunoglobulin domain

(type I and II)

NRG-IG_for NRG-TM_rev

GCCAGGGAAGTCAGAACTTC GTTTTGCAGTAGGCCACCAC

543

Glycosylation sites (type I) NRG-Glyc_for

NRG-TM_rev

CCACAGAAGGAGCAAATACTTC GTTTTGCAGTAGGCCACCAC

339

NRG-Kringle_rev

AGGAGGAGGAGTGGTGCTG GTCCCCAGCAGCAGCAGTA

239

Cysteine rich domain (type III) NRG-CRD_for

NRG-CRD_rev

GAGGTGAGCCGATGGAGATTTA CCTCTCAGGCGCTCAGCTTC

219

NRG-a_rev

TCTCCGGCGAGATGTCCGA GCTCCAGTGAATCCAGGTTG

668

NRG-Beta_rev

TCTCCGGCGAGATGTCCGA GGCAGCGATCACCAGTAAAC

677

GAPDH_rev

GAAGGGCTCATGACCACAGTCCAT TCATTGTCGTACCAGGAAATGAGCTT

450

Fig 2 Proteolytical processing of APP and NRG-1 in U373 cells U373 cells overexpressing human APP695 were incubated with inhibitors for b-secretase, c-secretase or metalloproteinases, or stimulated with phorbol 12-myristate 13-acetate Proteolytic processing products of APP or NRG-1 were detected in culture supernatants after precipitation or in lysed cells with appropriate antibodies (A) Cells were incubated with the tripeptidic inhibitor of the b-secretase (25 l M ) and shedded APPs-b or NRG-1 was visualized by western blotting (B) Full length pro-tein (FL) or C-terminal membrane tethered fragments (CTF) of either APP or NRG-1 were detected in cell lysates after an incubation period

of 48 h with 2 l M DAPT (C) Phorbol 12-myristate 13-acetate (PMA) (1 l M , 4 h) or GM6001 (10 l M , 26 h) were added to the cells to investi-gate the influence of metalloproteinases on secretion of NRG-1 ectodomain (NTF, N-terminal fragment) in U373 cells APPs-a served as a control All blots show samples from solvent-treated cells in lanes 1 and 3, whereas lanes 2 and 4 show samples from compound-treated cells Blots are representative for at least three independently performed experiments per treatment Quantifications display the mean ± SD; values from solvent-treated cells were set to 100% (Student’s t-test: ***P < 0.001; **P < 0.01; *P < 0.05).

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Proteolytical processing of NRG-1 in the human

astroglioma cell line U373

The tripeptidic b-secretase inhibitor II led to an 80%

reduction of soluble b-secretase cleaved APP (APPs-b)

in cell culture supernatants and also diminished

signifi-cantly the 60 kDa soluble NRG-1 in cell conditioned

medium (N-terminal fragment; Fig 2A) Furthermore,

the c-secretase inhibitor

N-[N-(3,5-difluorophenacetyl)-l-alanyl ]-S-phenylglycine t-butyl ester (DAPT), which

induced accumulation of C-terminal fragments of APP

in cell lysates (C-terminal fragment; Fig 2B), increased

the NRG-1 C-terminal fragment of approximately

50 kDa six-fold as compared to solvent-treated cells

These results demonstrate cleavage of NRG-1 in U373

cell line by both b- and c-secretase

Phorbol 12-myristate 13-acetate, a known inducer of

shedding events, significantly elevated soluble APPs-a,

as well as the soluble N-terminal fragment of NRG-1

in those cells, by 200% and 150% (Fig 2C) For this

reason, we analyzed metalloproteinase dependent

shed-ding of NRG-1: APPs-a that acted as a control was

reduced to 40% by the broad spectrum

metalloprotein-ase inhibitor GM6001 as compared to solvent-treated cells, and NRG-1 cleavage also was reduced signifi-cantly, although to a lower extent (65% of control cells; Fig 2C) Therefore, metalloproteinases appear to

be involved in NRG-1 processing in the astrocytoma cell line U373, as previously described for other cell lines [28,55]

RNA interference (RNAi)-induced knockdown of ADAM10 has no influence on NRG-1 shedding Because GM6001, which was used for inhibitory stud-ies, is a broad spectrum inhibitor of MMPs as well as ADAMs, we chose the RNAi approach to analyze in particular the role of ADAM10 in NRG-1 cleavage As

a control for unspecific RNAi-induced effects, MMP2 knockdown was examined as well RNAi treatment tar-geted against endogenous ADAM10 of the U373 cells resulted in a 60% reduction of mature ADAM10, whereas MMP2 targeted oligomers had no influence (Fig 3A) The decrease of ADAM10 due to RNAi was accompanied by a 30% decrease in APPs-a shedding (Fig 3B) serving as an internal control Because APP is

Immature Mature

Fig 3 Influence of siRNA mediated knock-down of ADAM10 on APP or NRG-1 processing in U373 cells U373 cells were transfected with a set of RNA oligomers targeted to ADAM10 (AD)

Mock-transfect-ed cells (C) or cells transfectMock-transfect-ed with RNA oligomers against MMP2 (M) were used as controls Forty-eight hours after transfection, cells were investigated with respect to ADAM10 and products of APP or NRG-1 proteolysis (A) The mature and immature forms of ADAM10 in the cell lysates were detected by western blotting and the mature, catalytically active form of the enzyme was quantified (B) APPs-a was enriched by trichloroacetic acid precipitation and visualized by the specific antibody 6E10 (C) Secreted (NTF, N-terminal frag-ment) and membrane bound NRG-1 species (CTF, C-terminal fragment) were detected in cell supernatants or lysates All western blottings show two sets of independent samples Quantifications are based on four independent experiments and show the mean ± SD; values from mock-transfected cells were set to 100% (one-way analysis of variance ⁄ Bonferroni post hoc test:

***P < 0.001; **P < 0.01).

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not only a substrate for ADAM10, but also, for

exam-ple, TACE, the absolute effect of ADAM10 knockdown

was small but reached significance By contrast, for

NRG-1, we observed no alteration of soluble NRG-1 in

cell culture supernatants, as well as for the

membrane-bound protein species Because of a potential

compensa-tion of reduced NRG-1 cleavage by other secretases, we

cannot exclude the possibility that ADAM10 might

have an effect on proteolytic processing of NRG-1 in

U373 cells but, if this is the case, ADAM10 at least is

not a major sheddase of this protein (Fig 3C)

In vivo effect of ADAM10 on NRG-1 proteolysis

Because ADAM10 was not implicated in the shedding

of distinct NRG-1 isoforms of cultured human

astro-glioma cells (a2 and b2; Fig 1B), we analyzed NRG-1

processing in ADAM10 overexpressing mice to take

into account all of the expressed isoforms Two

trans-genic mouse lines with different expression levels of

ADAM10 (moderate, ADAM10mo; high, ADAM10hi)

and a mouse line transgenic for a dominant negative

ADAM10 mutant (ADAM10dn) were included in this

investigation All mouse lines have been examined in

detail elsewhere with respect to APP processing,

learn-ing and behaviour [40,41,56] The expression of the proteinase itself is illustrated in Fig 4A (lower part)

In soluble protein fractions of brains derived from the three transgenic lines, the amount of the N-terminal fragment of NRG-1 (approximately 60 kDa; Fig 4) was not changed compared to the wild-type Addition-ally, neither full length NRG-1, nor C-terminal frag-ments in the brain membrane fraction were influenced

by an altered ADAM10 amount or activity (Fig 4)

We therefore conclude that, in vivo, the proteolytic processing of NRG-1 does not depend on the a-secre-tase ADAM10

For further confirmation of these findings, we exam-ined the myelination of peripheral nerves in ADAM10 transgenic mice and mice overexpressing dominant negative ADAM10 Because myelination strongly depends on NRG-1-ErbB signalling of Schwann cells and neurones [57], any relevant change of this pathway induced by altered ADAM10 activity should be obser-vable as a physiological consequence Again, the ADAM10 transgenes remained without effect in all investigated mouse lines (Fig 5A) G-ratios of ADAM10mo as well as of ADAM10dn mice at postnatal day 17 were identical to nontransgenic litter-mates Furthermore, Akt-phosphorylation, which also

Fig 4 Processing products of NRG-1 in ADAM10 transgenic mice Soluble and membrane tethered fractions of NRG-1 from brains of ADAM10mo, ADAM10hi and ADAM10dn mice were detected by western blotting with antibodies against the N- (NT) or the C-terminus (CT)

of the protein Nontransgenic littermates (Wt, wild-type) were used as controls Each western blot for NRG-1 shows samples from two indi-viduals: lanes 1 and 3 are from wild-type animals and lanes 2 and 4 are from transgenic mice For ADAM10 (detection by HA-antibody), one exemplary blot from the brain membrane fraction of four individuals is shown The proform of the proteinase is indicated by a black arrow head and the catalytically active form is indicated by a grey arrow head (B) Protein bands with respect to shedded (N-terminal fragment; 60 kDa) or one exemplary C-terminal fragment (50 kDa) of NRG-1 were quantified and values from wild-type mice were set to 100% (mean ± SEM; n = 6 for each mouse line, P > 0.05).

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Fig 5 ADAM10 transgenic mice display no disturbance in peripheral myelination (A) Sciatic nerves of ADAM10mo, ADAM10dn and wild-type (Wt) mice (postnatal day 17) were analyzed for myelin sheath thickness by electron microscopy Two exemplary microscopic images are shown for each mouse line G-ratios were evaluated taking into account at least 350 individual axons per group (n = 3 animals for each group) (B) Myelination was analyzed in adult, aged ADAM10hi mice (15–17 months) in analogy to (A) Two electron microscopy images at two different magnifications (see scale bars) of transgenic mice and age-matched control mice are shown Tomacula-like structures are indicated by black arrows.

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is partly controlled by NRG-1 signaling [31,58,59], was

unaffected in both mouse lines (Fig 6) In adult mice

with a high expression level of ADAM10

(ADAM10hi), G-ratios were also unaltered (Fig 5B),

but tomacula-like structures (local myelin thickenings

[60]) were observed Additionally, in the mouse line

with higher ADAM10 expression (ADAM10hi),

Akt-phosphorylation was significantly reduced to 40%

compared to wild-type mice This probably reflects

effects that do not depend on NRG-1 cleavage

Discussion

The data obtained in the present study for the human

astroglioma cell line U373 clearly reveal BACE-1 and

c-secretase dependent shedding of the endogenous

ErbB receptor ligand, which we identified

predomi-nantly as type a2-NRG-1 and, to a lesser extent, as the b2 isoform Additionally, GM6001, a broad spec-trum metalloproteinase inhibitor, was able to reduce NRG-1 shedding but a specific knockdown of ADAM10 by RNAi remained without any effect within the cellular system Therefore, the present study demonstrates that ADAM10 is not a major sheddase

of neuregulin-1 and enhancement of ADAM10 will probably have no side effects due to NRG-1 cleavage Because catalytically active ADAM10 is found on the plasma membrane [38] and neuregulin-1b1 cleav-age, for example, is restricted to the Golgi apparatus [28], it is plausible that distinct localization of ADAM10 and NRG-1 might inhibit a functional sub-strate–proteinase interaction Furthermore, NRG-1 is mainly found in cholesterol rich lipid rafts [61,62], favouring its role as a BACE-1 substrate, whereas ADAM10 and its catalytic activity (at least for APP) were shown to be localized in cholesterol-poor nonraft regions of the membrane [39] Nevertheless, a possible

in vivo relevance of ADAM10 to NRG-1 shedding required investigation due to the fact that NRG-1 pro-teolysis also depends on, for example, electric stimula-tion of cells [8], which might be accompanied by translocation within the cell Furthermore, the animal model offers a more complex representation because of the wide variety of cells that express NRG-1 and which might interact

Reconstitution experiments with transfection of ADAM10 in ADAM17) ⁄ ) embryonic mouse fibro-blasts [55] suggested only a minor influence of ADAM10 on neuregulin-1 shedding, but any positive proof in the living animal was still missing Therefore,

we investigated neuregulin-1 processing in mice with postnatal expression of ADAM10 or its dominant neg-ative variant The Thy.1-promoter driven expression of both ADAM10-constructs [40] occurs at postnatal day 1 (data not shown) Thy.1-based expression in general is predominantly found in postmitotic neuro-nes of the perinatal period, but also occurs in dorsal root ganglia and in spinal cord [63] Hence, the animal model is sufficient to study early ontogenetic phenom-ena after birth without disturbances due to impeded embryonic development in the central or peripheral nervous systems

In a recent study, the age-dependency of NRG-1 cleavage by BACE-1 was demonstrated [64] Although the accumulation of full length neuregulin-1 in BACE) ⁄ ) mice aged 15 days confirmed previous data [29,34], mice at postnatal day 30 or even older (2 years) showed no abnormalities with respect to neu-regulin-1 processing In the case of ADAM10, investi-gations of adult mice moderately overexpressing

Fig 6 Akt-phosphorylation in ADAM10 transgenic mice (A)

Total-Akt and phospho-Total-Akt were detected by western blotting in soluble

fractions of brains from ADAM10mo, ADAM10hi and ADAM10dn

mice Nontransgenic littermates (Wt, wild-type) were used as

con-trols (B) Phospho-Akt was normalized by total-Akt and quotients

from wild-type mice were set to 100% Values represent

the mean ± SEM (n = 4 for each mouse line; one-way analysis of

variance ⁄ Bonferroni post hoc test: **P < 0.01).

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ADAM10 or its dominant negative variant resulted in

totally unchanged amounts of NRG-1 processing

products

Therefore, the influence of ADAM10 on NRG-1 was

additionally analyzed in young mice (postnatal day 17)

by the status of peripheral nerve ensheathment In the

second postnatal week, myelination is almost finished in

mice (central nervous system [65]; peripheral nervous

system [66]); therefore, alterations should be apparent

However, neither moderate ADAM10 overexpressing

mice, nor mice with a restriction of enzyme activity by

dominant negative ADAM10, revealed differences in

axon myelination parameters compared to wild-type

littermates at postnatal day 17

Surprisingly, adult mice with high levels of

ADAM10 overexpression showed myelin infoldings

(tomacula-like structures) This observation has not

been made in the context of reduced or enhanced

NRG-1 signalling in mice [67] We therefore suggest

that mechanisms beside NRG-1 signal transduction

might be responsible for the neuropathological

pheno-type It will be interesting to analyze these

observa-tions in future studies

Additionally, Akt phosphorylation, a consequence

of NRG-1-ErbB signalling [31,59], was unaltered by

moderate overexpression or by inhibiting ADAM10

activity by its negative mutant form However, mice

with high overexpression of ADAM10 showed a strong

decrease of phosphorylated Akt compared to

non-transgenic mice This observation may relate to recent

findings demonstrating that a high level of ADAM10

overexpression in the mouse increases susceptibility to

kainate-induced seizures and neuronal damage [56],

whereas the neuroprotective properties of ADAM10

were only evident in mice with APP overexpression

In conclusion, ADAM10 was excluded both in cell

culture and in the animal model as a major candidate

secretase for neuregulin-1 shedding We cannot rule

out that other secretases, such as TACE or ADAM19,

which were identified formerly as NRG-1 sheddases

[28,30,55], compensate for the lack of ADAM10 in

RNAi-treated cells or animals with overexpression of

the dominant negative mutant In breast cancer cells,

ADAM10 was described to mediate the shedding of

the receptor ErbB2 [68]; therefore, an influence on

NRG-1-ErbB signalling could in principal have also

occurred by ErbB2 cleavage in our transgenic mice

However, because we did not observe an influence on

myelination in ADAM10 transgenic mice, this

observa-tion might be restricted to tumour cells

We also cannot exclude that, in non-neuronal

tis-sue, embryonic development or pathological stages

ADAM10 itself, or cleavage products of its other

sub-strates, might be involved in NRG-1-ErbB cross-talk

In summary, however, we present evidence demonstrat-ing that, in the healthy early postnatal and adult mouse, moderate alterations in the amount of ADAM10 do not interfere with neuregulin-1 signalling Accordingly, ADAM10 will have no impact on down-stream physiological functions such as nerve remyelina-tion or the schizophrenia-resembling psychiatric changes as observed for BACE-1 knockout mice [34,69] The results obtained in the present study there-fore suggest that a moderate upregulation of ADAM10 expression and its a-secretase activity with a preventive

or therapeutical intention is not impaired by side effects resulting from the NRG-1-ErbB signalling network

Experimental procedures

Antibodies, inhibitors and RNAi oligomers

The primary antibodies used were: 6E10 for the detection

of APPs-a (Senetek, St Louis, MO, USA; dilution

1 : 1000), anti-neuregulin-1 (H-210; dilution 1 : 200) for the detection of secreted NRG-1 fragments, anti-neuregulin-1a⁄ b1 ⁄ 2 (C-20; dilution 1 : 500) (both Santa Cruz Biotech-nology, Santa Cruz, CA, USA) for the detection of membrane bound NRG-1, anti-ADAM10 (Chemicon, Temecula, CA, USA; dilution 1 : 1000) for the detection of the proteinase in cells and 6687 (C Haass, LMU Munich, Germany) for the detection of full length APP and C-termi-nal protein fragments Anti-P-Akt and anti-total Akt were purchased from Cell Signaling [PhosphoPlus Akt (Ser473) Antibody Kit; Cell Signaling, Danvers, MA, USA] Overex-pressed ADAM10 in mouse brain membranes was visual-ized by HA-antibody Y-11 (Santa-Cruz Biotechnology) The secondary antibodies were coupled to alkaline phos-phatase (Tropix, Bedford, MA, USA; dilution 1 : 10000) or horseradish peroxidase (Pierce, Rockford, IL, USA; dilution 1 : 3000) and were used in combination with their substrates CDP-Star (Tropix) or SuperSignalECL (Pierce) The b-secretase-inhibitor II (Calbiochem, Bad Soden, Germany) was applied at a concentration of 25 lm and the c-secretase inhibitor DAPT (B Schmitt, Clemens Scho¨pf-Institute of Organic Chemistry and Biochemistry, Tech-nische Universita¨t Darmstadt, Germany) was applied at a concentration of 2 lm GM6001 (Calbiochem, San Diego,

CA, USA) was used at a final concentration of 10 lm and phorbol 12-myristate 13-acetate (Sigma, Deisenhofen, Ger-many) was used at a concentration of 1 lm All substances were dissolved in dimethylsulfoxide as stock solutions For the RNAi experiments, the Stealth RNAis ADAM10 HSS165, HSS166, HSS167 and MMP2 HSS106612, HSS106613, HSS106614 (Invitrogen, Karlsruhe, Germany) were used Transfections were performed with Opti-MEM and Lipofectamine2000 (Invitrogen)

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RNA preparation and RT-PCR

The RNA of U373 cells was isolated by using confluent 6 cm

culture plates and the RNA isolation kit with on-column

DNA digestion as recommended in the manufacturer’s

pro-tocol (Macherey-Nagel, Du¨ren, Germany) Four hundred

nanograms of RNA were reverse transcribed in a 20 lL

reac-tion volume by the reverse-it-RT-PCR-kit from ABgene

(Hamburg, Germany) with intron-spanning specific primers

(0.2 lm each) Amplificates were analyzed on 1% agarose

gels and GAPDH amplification served as a control for the

RT-PCR reaction and PCR conditions Primer sequences

and the amplificate length are provided in Table 1

The amplificates from RT-PCR with primers

NRG-jD_for and NRG-TM_rev were ligated into pUC19

(Fer-mentas, St Leon-Rot, Germany) and plasmid DNA from

eight positive clones (identified by blue–white selection) was

sequence analyzed with M13 universal primer

Preparation of mouse brain samples

The generation of transgenic mice has been described

previously [40] Seven- to 10-week-old mice were sacrificed,

the brains were dissected and stored on dry ice Ice-cold

Tris buffer (20 mm Tris⁄ HCl, pH 8.5) containing proteinase

inhibitors (Inhibitor Complete Mini; Roche Diagnostics

Corp., Mannheim, Germany) was added and tissue was

homogenized in a tissue lyser (Eppendorf, Hamburg,

Ger-many) with a frequency of 20 Hz for 2 min The

superna-tants resulting from centrifugation at 13 500 g for 1.75 h

were used for the detection and quantification of soluble

NRG-1 NRG-1 membrane bound full length protein and

membrane bound NRG-1 fragments, as well as the

protein-ase ADAM10 itself, were detected in the membrane

frac-tions prepared from centrifugation pellets

For total-Akt and phospho-Akt detection, brain

hemi-spheres were homogenized in lysis buffer supplemented with

additional phosphatase inhibitors (2.5 mm

Na-pyrophos-phate, 1 mm b-glycerophosphate and 1 mm Na3VO4) and

soluble proteins were isolated from membrane fractions by

centrifugation at 20 800 g for 20 min

Cell culture, treatment with inhibitors and RNAi

silencing

U373 cells overexpressing human wild-type APP were

main-tained in MEM (Sigma, Taufkirchen, Germany)

supple-mented with 10% fetal bovine serum, 1% sodium pyruvate

and 1% glutamine

To inhibit b-secretase or metalloproteinases, cells were

pretreated with the appropriate inhibitor

(b-secretase-inhibi-tor II or GM6001) for 22 h Then, the serum containing

culture medium was removed and medium without serum

supplemented with fatty acid free BSA (1 mgÆmL)1) and

fresh inhibitor was added for an additional 4 h Phorbol 12-myristate 13-acetate-induced shedding was performed for 4 h in serum free BSA supplemented medium For inhi-bition of c-secretase, cells were treated with DAPT for 48 h

in culture medium

For RNAi experiments, cells were transfected with

750 pmol of RNAi oligomers (250 pmol each) in six-well plates After 5 h of transfection, the medium was replaced

by culture medium After 44 h, cells were covered with serum-free medium and incubated for 4 h for collection of secreted proteins and cell lysates

Western blotting

Proteins of cell culture supernatants were precipitated with trichloroacetic acid and normalized by the protein content

of the cell lysates Adequate amounts of soluble or mem-brane tethered proteins were separated on 8% SDS-gels or 4–12% Bis–Tris NuPAGE gels (Invitrogen) and blotted on

a poly(vinylidene difluoride) membrane or nitrocellulose (total-Akt and phospho-Akt) Proteins were then detected with the appropriate primary antibodies Chemiluminescent signals from alkaline phosphatase or horseradish peroxidase coupled secondary antibodies were visualized with a charge-coupled device camera and the software versa doc (Bio-Rad, Munich, Germany) and were quantified with aida3.5 (Raytest, Straubenhardt, Germany)

Electron microscopy and G-ratio determination

Seventeen-day-old or adult transgenic mice (15–17 months old) and nontransgenic littermates were perfused with NaCl⁄ Picontaining 60 lgÆmL)1 heparin followed by 2.5% glutaraldehyde⁄ 4% parafomaldehyde in 0.1 m phosphate buffer Afterwards, sciatic nerves were removed, postfixed and contrasted with osmium tetroxide and processed for electron microscopy [70] biovision software (Soft Imaging System GmbH, Mu¨nster, Germany) was used for determi-nation of the G-ratio by measuring the inner and outer myelinated fibres

All animal procedures were performed according to the German guidelines for the care and the use of laboratory animals and in accordance with the European Communities Council Directive of 24 November 1986 (86/609/EEC)

Acknowledgements

We thank C Griffel (MDC, Berlin) for excellent tech-nical support in the analysis of sciatic nerve myelina-tion; A Schro¨der (ZVTE, Mainz) for coordination of animal husbandry and M Willem (LMU, Munich) for fruitful discussion This work was supported by grants from the DFG priority program 1040 (to F.F.)

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