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Arsenite stimulated glucose transport in 3T3-L1 adipocytes involves both Glut4 translocation and p38 MAPK activity Merlijn Bazuine, D.. These data show that in 3T3-L1 adipocytes both ars

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Arsenite stimulated glucose transport in 3T3-L1 adipocytes involves both Glut4 translocation and p38 MAPK activity

Merlijn Bazuine, D Margriet Ouwens, Daan S Gomes de Mesquita and J Antonie Maassen

Department of Molecular Cell Biology, Leiden University Medical Centre, Leiden, the Netherlands

The protein-modifying agent arsenite stimulates glucose

uptake in 3T3-L1 adipocytes In the current study we have

analysed the signalling pathways that contribute to this

response By subcellular fractionation we observed that

arsenite, like insulin, induces translocation of the GLUT1

and GLUT4 glucose transporters from the low-density

membrane fraction to the plasma membrane Arsenite did

not activate early steps of the insulin receptor (IR)-signalling

pathway and the response was insensitive to inhibition of

phosphatidylinositol-3¢-kinase (PI-3¢) kinase by

wortman-nin These findings indicate that the ÔclassicalÕ

IR–IR substrate–PI-3¢ kinase pathway, that is essential for

insulin-induced GLUT4 translocation, is not activated by

arsenite However, arsenite-treatment did induce

tyrosine-phosphorylation of c-Cbl Furthermore, treatment of the

cells with the tyrosine kinase inhibitor, tyrphostin A25,

abolished arsenite-induced glucose uptake, suggesting that

the induction of a tyrosine kinase by arsenite is essential for

glucose uptake Both arsenite and insulin-induced glucose

uptake were inhibited partially by the p38 MAP kinase inhibitor, SB203580 This compound had no effect on the magnitude of translocation of glucose transporters indica-ting that the level of glucose transport is determined by additional factors Arsenite- and insulin-induced glucose uptake responded in a remarkably similar dose-dependent fashion to a range of pharmacological- and peptide-inhibi-tors for atypical PKC-k, a downstream target of PI-3¢ kinase signalling in insulin-induced glucose uptake These data show that in 3T3-L1 adipocytes both arsenite- and insulin-induced signalling pathways project towards a similar cel-lular response, namely GLUT1 and GLUT4 translocation and glucose uptake This response to arsenite is not func-tionally linked to early steps of the IR–IRS–PI-3¢ kinase pathway, but does coincide with c-Cbl phosphorylation, basal levels of PKC-k activity and p38 MAPK activation Keywords: PKC-k; PKB; PI-3¢ kinase; insulin; Cbl

Insulin induces multiple responses in target tissues such as

adipocytes and muscle through the intracellular activation

of several signal transduction pathways These responses

include a pronounced anabolic action on protein and lipid

metabolism, an antiapoptotic response, an increase in

glucose uptake, and stimulation of glycogen synthesis

[1,2] Insulin-stimulated glucose uptake occurs primarily

via translocation of the GLUT4 glucose transporter to the

plasma membrane [3,4] This process is initiated by the

activation of the insulin receptor (IR) tyrosine kinase

followed by receptor autophosphorylation and tyrosine

phosphorylation of downstream effectors like insulin

receptor substrate-1 (IRS-1), IRS-2 and related proteins

Tyrosine phosphorylated IRS proteins provide docking

sites for class I phosphatidylinositol-3¢ (PI-3¢) kinase that becomes activated upon binding to these proteins [5,6] Numerous studies have shown that PI-3¢ kinase activation provides an essential signal for the stimulation of glucose uptake by insulin [7,8] Downstream targets of PI-3¢ kinase

in 3T3-L1 adipocytes that have been implicated in signalling towards GLUT4 translocation are the AGC kinase family members PDK1, PKB and the atypical PKC-k/-f [9–11], of which 3T3-L1 adipocytes only express the k-isoform [12] Recent data also demonstrate the involvement of an additional, nonPI-3¢ kinase dependent pathway involving c-Cbl which becomes tyrosine-phosphorylated upon APS (adapter protein with a PH and SH2 domain)-mediated association with the activated insulin receptor [13] Sub-sequently, tyrosine-phosphorylated c-Cbl translocates towards the caveolae and induces the activation of the small GTP-binding protein, TC10 [14], ultimately signalling towards the exocyst complex (Exo70) involved in GLUT4 translocation [15]

Apart from insulin, some other stimuli, like muscle contraction, H2O2 and hyperosmotic shock, have been shown to stimulate GLUT4-mediated glucose uptake in adipocytes and muscle Most studies show that these stimuli are not sensitive to inhibition by wortmannin, indicating PI-3¢ kinase is not involved in glucose uptake mediated by these agents [16–18]

Sodium arsenite is known for its atherogenic, carcino-genic and genotoxic effects Recently, arsenite has also

Correspondence to J A Maassen, Department of Molecular Cell

Biology, Leiden University Medical Centre, Wassenaarseweg 72,

PO Box 9503, 2333 AL, Leiden, the Netherlands.

Fax: + 31 71 5276437, Tel.: + 31 71 5276127,

E-mail: J.A.Maassen@lumc.nl

Abbreviations: IR(s), insulin receptor (substrates); IBMX,

1-methyl-3-isobutylxanthine; PI-3¢, phosphatidylinositol-3¢-kinase;

2-DOG, 2-deoxy- D [ 14 C]glucose; BIM I, bisindolylmaleimide I;

LDM, low density microsome; PM, plasma membrane;

TPA, 12-O-tetradecanoylphorbol 13-acetate.

(Received 18 December 2002, revised 24 July 2003,

accepted 28 July 2003)

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been used effectively as a chemotherapeutic drug in the

treatment of acute promyelocytic leukaemia patients

[19,20] At the protein level, arsenite exerts its biological

effects through modification of vicinal sulfhydryl groups

in specific target proteins For instance, arsenite

specific-ally inactivates the E2 subunit of branched-chain

alpha-keto acid dehydrogenase (but not the other subunits) [21]

and activates heat shock protein 70 [22] Arsenite is also a

potent activator of the stress kinases, JNK and p38, by

modulating the activity of an unidentified target protein

[23] Furthermore, arsenite has been shown to induce

glucose uptake in 3T3-L1 adipocytes, baby hamster

kid-ney cells and L6 muscle cells [24–26] As the action of

arsenite involves the modification of a limited number of

arsenite-sensitive target proteins, we hypothesized that

elucidation of the mechanism of arsenite-induced glucose

uptake may contribute to a better understanding of

insulin-induced glucose uptake

In this study, we observed that arsenite displays

insulin-like effects on GLUT4-mediated glucose transport in

adipocytes To explore the underlying mechanism we

analysed the signalling pathways that are activated by

arsenite in comparison to insulin and that contribute to

stimulation of glucose uptake

Experimental procedures

Materials Dulbecco’s modified Eagle’s medium (DMEM) was pur-chased from Life Technologies, Inc.; foetal bovine serum was from Brunschwig, Amsterdam; bovine insulin, 1-methyl-3-isobutylxanthine (IBMX), dexamethasone, 12-O-tetradecanoylphorbol 13-acetate (TPA) and 2-deoxy-glucose were obtained from Sigma 2-deoxy-D-[14C]glucose was purchased from NEN-Dupont Tyrphostin A25, SB203580, chelerythrine chloride, bisindolylmaleimide I, Go¨ 6976, Ro 31-8220 and Ro 32-0432 were from Calbio-chem LY-294002, microcystin LR and wortmannin were obtained from Alexis Myristoylated pseudosubstrate pep-tide inhibitors for PKC-a/-b and PKC-k/-f were purchased from Biomol For an overview of the characteristics of the pharmacological inhibitors applied in this study, see Table 1

Antibodies Polyclonal antisera recognizing IRS-1, and the regulatory subunit of PI-3¢ kinase were described previously [27] Table 1 Characteristics of pharmacological inhibitors applied in this study.

Pharmacological inhibitor Concentration applied Described target IC 50 Reference

MAPK activated protein-kinase 1b 50 n M [52]

Mitogen and stress activated kinase-1 <1 l M [53]

4 l M in vivo

[11] Glycogen synthase kinase 3b 38 n M

2.8 n M

[53] [50] MAPK activated protein-kinase 1b 3 n M [52]

Mitogen and stress activated protein kinase 8 n M [53]

a

Disputed by Davies et al [53].

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A polyclonal antiserum recognizing IRS-2 is described in

a recent paper from our group [28] HRP-conjugated

mouse monoclonal anti-(phosphotyrosine Ig) pY-20,

mouse monoclonal pY-20, rabbit polyclonal antibody

against PKC-k/-f (C-20) and polyclonal against Cbl

(C-15), goat polyclonal antibodies recognizing the

cata-lytic (p110a) subunit of PI-3¢ kinase (C-17) and GLUT4

(C-20) were obtained from Santa Cruz Biotechnology,

Inc Rabbit polyclonal antibody recognizing IRb-chain

and mouse monoclonal integrin b1, Cbl and PKC-k were

purchased from Transduction Laboratories The

phospho-specific antibodies recognizing PKC-k (T403), caveolin-1

(Y14), PKB (T308 and S473), MAPKAP-K2 (T334), p38

(T180/Y182) and ERK-1/)2 (T202/Y204) were obtained

from Cell Signalling Technology Sheep polyclonal

anti-body recognizing PKB was purchased from Upstate

Biotechnology The rabbit polyclonal antibodies against

GLUT-1 and -4 (used in the PM-lawn assay) have been

described [29] The appropriate HRP- and

FITC-conjugated secondary antibodies were obtained from

Promega

Cell culture

3T3-L1 Fibroblasts, obtained from American Type

Cul-ture Collection (Manassas, VA, USA), were culCul-tured and

differentiated to adipocytes as described previously [30]

Cells were routinely used 7 days after completion of the

differentiation process, with only cultures in which >95%

of cells displayed adipocyte morphology being used Prior to

use, adipocytes were serum starved for 16 h with DMEM

supplemented with 0.5% foetal bovine serum

Membrane isolation assay

3T3-L1 adipocytes were stimulated as indicated in the figure

legends Subsequently cells were washed twice in ice-cold

HES buffer (20 mM Hepes pH 7.4, 1 mM EDTA and

250 mMsucrose) on ice and scraped in HES buffer in the

presence of protease inhibitors (complete protease inhibitor

cocktail, Boehringer Mannheim) Samples were

homogen-ized by nine times three strokes in a glass potter

homo-genizer after which low density microsome (LDM) and

plasma membrane (PM) fractions were isolated by

differ-ential centrifugation as described by Simpson et al [31]

Equal amounts of protein as determined with BCA

protein assay reagent (Pierce) were subjected to immunoblot

analysis using various antibodies

Plasma membrane-lawn assay

The plasma membrane-lawn assay was performed as

described previously [32] Digital fluorescence imaging was

performed using a Leica DM-RXA epifluorescence

micro-scope (Leica, Germany) equipped with a 100-W mercury

lamp and the appropriate filters

Assay of 2-deoxyglucose uptake

3T3-L1 adipocytes, grown in 12-well plates (Costar), were

subjected to an assay of 2-deoxy-D-[14C]glucose (0.075 lCi

per well) uptake as described previously [33]

Immunoprecipitations and Western blotting Dishes (9 cm) of 3T3-L1 adipocytes were stimulated with agonists Immunoprecipitation and immunoblotting pro-cedures were as described previously [27] For c-Cbl immunoprecipitation 9-cm dishes of 3T3-L1 adipocytes were stimulated with agonists and scraped in lysis buffer (1 mM Na3VO4, 1 mM EGTA, 1 mM EDTA, 50 mM

Tris/HCl pH 7.4, 1% NP-40, 0.5% sodium deoxycholate,

150 mM NaCl, 5 mM NaF in the presence of protease inhibitors) Cell lysates were tumbled for half an hour at

4C, cell lysate was cleared from cellular debris by spinning

at 14 000 g, for 10 min at 4C in a table-top centrifuge About 1 mg of cell lysate was subjected to immunopreci-pitation using 5 lg of anti-Cbl mouse monoclonal 7G10 (UBI) for 1.5 h at 4C Immunocomplexes were harvested

by incubating with ProtGbeads for 1.5 h at 4C Beads were washed in lysis buffer and dissolved subsequently in sample buffer Phosphotyrosine was demonstrated by immunoblotting using anti-pY20 followed by anti-(mouse HRP) secondary Ig Immunoblots were quantified using

LUMIANALYST software on a LumiImager (Boehringer-Mannheim)

PI-3¢ kinase activity assay Dishes (9 cm) of 3T3-L1 adipocytes were stimulated with agonists and immunoprecipitated using time, concentration and antibodies as indicated in the figure legends Cells were lysed and IRS-1 and p85 immunoprecipitates collected on protein A–Sepharose beads were analysed for the copreci-pitation of in vitro PI-3¢ kinase activity using 5 lCi c-32 P-labelled ATP per reaction as described by Burgering et al [34] Incorporated radioactivity was quantified on a Molecular Dynamics phosphorimager

PKC-k kinase assay Dishes (9 cm) of 3T3-L1 adipocytes were stimulated with

100 nMof insulin for 10 min or 0.5 mMarsenite for 30 min Cells were lysed in an NP-40 based lysis buffer (see above) in the presence of 1 lM microcystin LR and immunopreci-pitated with 5 lg mouse monoclonal PKC-k for 1.5 h at

4C Subsequently, Prot-Gbeads were added and com-plexes were harvested after another 1.5 h The precipitate was washed three times with lysis buffer and two times with kinase assay buffer (100 mMHepes pH 7.4, 10 mMMgCl2,

1 mM dithiothreitol) PtdSer (4 lg per sample) was dried under N2(g)and dissolved in 25 lL kinase buffer per sample Subsequently, PtdSer was waterbath-sonicated three times for 5 min and 25 lL sample kinase buffer, ATP (40 lM, final concentration), 5 lCi c-32P-labelled ATP per reaction, dithiothreitol (1.5 mM), PKI (1 mM), the indicated concen-trations of Ro 31-8220, and PKCe-substrate (40 lM) were added As a control, 10 lM of a peptide identical to the PKC-k pseudosubstrate domain was added to determine the specificity of the assay Kinase reactions were allowed

to proceed for 10 min at 37C under gentle agitation Twenty microlitres of each reaction was spotted on p81 paper and washed three times for 5 min with 0.85% (v/v) phosphoric acid, and once for 5 min with acetone P81 papers were air dried and analysed in a scintillation counter

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Statistical analyses

Data were analysed with an independent-samples t-test

usingSPSS10.0 Curves represent fits to data by nonlinear

regression analysis usingGRAPHPAD PRISM2.01

Results

Arsenite induces 2-DOG uptake, GLUT1 and GLUT4

translocation in 3T3-L1 adipocytes

Incubation of 3T3-L1 adipocytes with arsenite stimulated

the uptake of hexose in a time- and dose-dependent manner

Stimulation of 2-deoxy-D[14C]glucose (2-DOG) uptake was

maximal at a 30-min preincubation period with 0.5 mM

arsenite (Fig 1A,B) On average, maximal stimulation of

glucose uptake was approximately sevenfold for insulin and

threefold for arsenite When insulin was added to adipocytes

during the final 15 minutes of a 30-min incubation with

arsenite, no significant additive response was seen on

arsenite-induced glucose uptake (Fig 1C) Under these

conditions, insulin did induce tyrosine phosphorylation of

IRb, IRS-1 and IRS-2, indicating that arsenite does not

interfere with the insulin-induced activation of this pathway

(data not shown)

Insulin-stimulated glucose transport predominantly

involves GLUT4 translocation from an intracellular

microsomal compartment to the plasma membrane of

adipocytes along with some induction of GLUT1

trans-location To determine whether arsenite stimulates

GLUT1 and GLUT4 translocation, we fractionated

adipocytes into membrane (PM) and microsomal vesicle

(LDM) fractions Equal amounts of protein ( 10 lg)

were subjected to immunoblot analysis (Fig 2A,C)

Plasma membrane fractions were identified using

antibod-ies against the IR b-chain and integrin-b1 (data not

shown) As can be seen in Fig 2A, when probing the

fractions with an antibody against GLUT4, both

insulin-and arsenite-treatment resulted in a shift of GLUT4 from

the microsomal fractions towards the plasma membrane

fractions Figure 2C shows that insulin induces some

translocation of GLUT1 towards the plasma membrane,

as did arsenite, albeit at lower levels than insulin The

amounts of GLUT1 and GLUT4 in each fraction were

quantified and expressed as a relative amount of total

GLUT protein in these fractions Arsenite significantly

increases the amount of GLUT4 in the PM (Fig 2B),

albeit at a lower level than insulin With respect to

GLUT1, although a consistent increase in the amount of

GLUT1 translocating towards the plasma membrane was

observed this did not reach significant levels compared to

basal levels of GLUT1 in the PM (Fig 2D) Furthermore,

arsenite did not change the total amount of GLUT4 or

GLUT1 in 3T3-L1 adipocytes (data not shown) It should

be noted that both GLUT1 and GLUT4 are heavily

glycosylated and show heterogeneous mobility

An alternative method to investigate GLUT protein

translocation is the plasma-lawn assay In this analysis,

sonicated cells are probed with an antibody recognizing

GLUT1 or GLUT4 and subjected to immunofluorescnce

microscopy As can be seen in Fig 2E, both GLUT1 and

GLUT4 are present in PM-lawns at higher quantities

after arsenite treatment as compared to the unstimulated situation

Combined, these data indicate that arsenite-stimulated glucose uptake involves translocation of the GLUT1 and the insulin-responsive GLUT4 glucose transporter

The effect of arsenite on early events in insulin receptor signalling

To elucidate the signalling-pathways that contribute to arsenite-induced GLUT4 translocation, we examined

Fig 1 Arsenite induces glucose uptake in 3T3-L1 adipocytes in a dose-and time-dependent manner (A) 3T3-L1 adipocytes were stimulated with the indicated concentrations of arsenite for 30 min and assayed for 2-deoxy- D [14C]glucose (2-DOG) uptake (B) 3T3-L1 adipocytes were stimulated with 0.5 m M arsenite for the indicated times and assayed for 2-DOGuptake (C) 3T3-L1 adipocytes were stimulated as indicated with 100 n M insulin for 15 min (ins), 0.5 m M arsenite for

30 min (as), or 0.5 m M arsenite for 30 min combined with 100 n M

insulin added after 15 min (as/ins) and assayed for 2-DOGuptake Incorporated radioactivity was determined by liquid scintillation counting Values are mean ± SEM of at least four determinations;

*P < 0.05 compared to basal and P < 0.05 for as/ins compared

to ins.

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whether arsenite activates intermediates of the insulin

signalling-pathway Following stimulation of 3T3-L1

adi-pocytes with either insulin or arsenite, IR, IRS-1 and IRS-2

were immunoprecipitated and assessed for tyrosine

phos-phorylation by Western blotting As shown in Fig 3A–C,

no significant increase in tyrosine phosphorylation of either

IRb, IRS-1 or IRS-2 could be detected in response to

arsenite Under these conditions, stimulation with insulin

led to a pronounced tyrosine phosphorylation of these

proteins In agreement with the lack of IRS-tyrosine

phosphorylation in response to arsenite, no association of

the p85 or p110a subunits of PI-3¢ kinase with the IRS

proteins was detected, again in contrast to the situation seen

after insulin stimulation (Fig 3B) Treatment with arsenite

did not lead to phosphorylation of PKB on either Ser473 or

Thr308, nor of phosphorylation of PKC-k onT403 This

observation agrees with the absence of PI-3¢ kinase

activa-tion by arsenite in vivo (Fig 3D) Consistent with these

observations, no increase of in vitro PI-3¢ kinase activity

was observed in IRS-1 immunoprecipitates after arsenite

treatment (Fig 4A), nor did we find any arsenite-induced

stimulation of in vitro PI-3¢ kinase activity in

immuno-precipitates of PI-3¢ kinase (Fig 4B)

To investigate the possibility that basal PI-3¢ kinase activity in combination with arsenite-induced signals is needed to stimulate glucose uptake, we examined the effect

of the PI-3¢ kinase inhibitor, wortmannin, on arsenite-induced glucose uptake Using concentrations that fully inhibited insulin-induced glucose uptake, arsenite-induced glucose uptake was unaffected by wortmannin (Fig 4C) Similar data were obtained using LY-294002 (data not shown) These observations suggest that arsenite-induced glucose uptake occurs without the need for PI-3¢ kinase activity, a situation that is in marked contrast to insulin induced glucose uptake Another early target of insulin action, the activation of ERK-1, -2 was also not activated appreciably in response to arsenite-treatment either (Fig 3D)

The effect of arsenite on Cbl and caveolin-1 tyrosine phosphorylation

A recently described PI-3¢ kinase independent pathway involved in insulin-induced glucose uptake in 3T3-L1 adipocytes involves Tyr phosphorylation of c-Cbl and caveolin-1 mediated by the IR Remarkably, we found

Fig 2 Arsenite-treatment induces GLUT1 and GLUT4 translocation to the plasma membrane in 3T3-L1 adipocytes 3T3-L1 adipocytes were mock-treated (basal), stimulated for 15 min with 100 n M insulin (insulin/ins) or for 30 min with 0.5 m M arsenite (arsenite/as) (A) Adipocytes were fractionated and equal amounts of protein from both microsomal (LDM) and plasma membranes (PM) were analysed by immunoblot with anti-GLUT4 Igs (B) anti-GLUT4 levels in each fraction subjected to immunoblot analysis as in A were quantified using a LumiImager and expressed as a fraction of GLUT4 residing in either LDM or PM (C) Subcellular fractions as in (A) were also subjected to immunoblot analysis using antibodies against GLUT1 (D) GLUT1 levels in each fraction were quantified as in (B) and expressed as a fraction of GLUT1 residing in either LDM or PM The total amount of GLUT1 or GLUT4 in the HDM fraction did not alter during either arsenite- or insulin-treatment Data are expressed as mean ± SEM of at least three independent observations, *P < 0.05 compared to basal (E) 3T3-L1 adipocytes were mock-treated (none), stimulated for 15 min with 100 n M insulin (ins) or for 30 min with 0.5 m M arsenite (as) Adipocytes were subjected to PM-lawn analysis using antibodies against either GLUT1 or GLUT4 Data shown are a representative example of five independent observations for each condition.

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that arsenite did induce tyrosine-phosphorylation of both

c-Cbl (Fig 5B) and caveolin-1 (Fig 5A), in spite of the

absence of IR activation This observation suggests that

arsenite does induce an as of yet unidentified tyrosine

kinase activity in 3T3-L1 adipocytes To evaluate whether

this tyrosine kinase activity is required for arsenite-induced

glucose uptake, we applied the tyrosine kinase inhibitor,

tyrphostin A25 Insulin-induced IRS and caveolin-1

tyro-sine phosphorylation are attenuated, but still present after

pretreatment with tyrphostin A25 (Fig 5A)

Insulin-induced Cbl phosphorylation is even enhanced by

tyr-phostin (Fig 5B) In contrast, arsenite-induced Cbl

and caveolin-1 phosphorylation are strongly inhibited

(Fig 5A,B) In a glucose uptake assay, tyrphostin A25

attenuated insulin-induced glucose uptake, but completely

blocked arsenite-induced glucose uptake (Fig 5C) These

data illustrate the distinct nature of the insulin- (namely

the IR) and arsenite-induced tyrosine kinases, and

fur-thermore they suggest that tyrosine kinase activity is a

requirement for arsenite-mediated induction of glucose

uptake in 3T3-L1 adipocytes

The effect of the p38 MAPK inhibitor, SB203580,

on arsenite-induced glucose uptake

SB203580 is a pharmacological inhibitor of the MAP kinase

family member p38 and has been shown to inhibit insulin

induced glucose uptake by 3T3-L1 adipocytes and L6

muscle cells [35,36] Arsenite-treatment induced

p38-phos-phorylation on Thr180 and Tyr182, and phosp38-phos-phorylation of

MAPKAP-K2 on Thr334 (a direct target site of p38 MAP kinase activity [37]) Treatment with 10 lM SB203580 significantly inhibited arsenite-induced glucose uptake

as well as MAPKAP-K2 and p38-phosphorylation (Fig 6A,B)

In insulin-signalling, p38 MAPK has been implied in enhancing the intrinsic activity of the GLUT4 glucose transporter Thus, SB203580 has been shown to reduce induced glucose uptake without an effect on insulin-induced GLUT4 translocation [35] SB203580 had a similar

Fig 4 Arsenite-induced in vitro PI-3¢ kinase activity 3T3-L1 adipo-cytes were stimulated as indicated with 100 n M insulin for 5 min or 0.5 m M arsenite for 30 min Cell lysates were incubated for 3 h with polyclonal antiserum against IRS-1 (A), or against the 85-kDa regu-latory subunit of PI-3¢ kinase (B) Immunoprecipitates were washed and subsequently subjected to an in vitro PI-3¢ kinase assay Copre-cipitating PI-3¢ kinase activity was determined on a phosphorimager as the relative stimulation of [c- 32 P]ATP incorporation into phosphati-dylinositol standardized against untreated cells Data are expressed as the mean ± SEM of three observations, statistically significant com-pared to basal (*P < 0.05) (C) 3T3-L1 adipocytes were pretreated for

15 min with 100 n M wortmannin Subsequently, adipocytes were mock-treated (basal) or stimulated as indicated with 100 n M insulin for

15 min or with 0.5 m M arsenite for 30 min in the continued presence of the pharmacological inhibitor and assayed for 2-DOGuptake Data are expressed as mean ± SEM of at least six observations Statistically significant data when compared to the samples not treated with wortmannin are indicated (*P < 0.05).

Fig 3 The effect of arsenite on the activation status of early steps in

insulin-responsive signal-transduction pathways 3T3-L1 adipocytes

were stimulated as indicated with 100 n M insulin for 5 min or 0.5 m M

arsenite for 30 min Cell lysates were immunoprecipitated with anti-IR

(A), anti-IRS-1 (B), anti-IRS-2 (C) followed by immunoblot analysis

with anti-phosphotyrosine (ap-Tyr), anti-PI-3¢ kinase regulatory

sub-unit (ap85) or anti-PI-3¢ kinase catalytic subsub-unit (ap110a) as indicated.

Equal loading was confirmed using the respective antibodies used for

immunoprecipitation (D) Total cell lysate of adipocytes (10 lg)

sti-mulated as described above was analysed by immunoblot using

phosphospecific antibodies against T202/Y204 of ERK-1/2 (apERK),

T308 and S473 of PKB (apThr308 and apSer473), T403 of PKC-k

(apPKCk) or PKB (aPKB) as indicated.

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effect on arsenite-induced glucose uptake (Fig 6; compare

A with C,D) i.e a reduction in glucose uptake without a

reduction in GLUT4 translocation

The effect of pharmacological inhibitors

of PKC-isoforms on arsenite-induced glucose uptake Atypical PKC isoforms (PKC lambda and zeta) have been implicated in insulin induced glucose uptake in adipocytes [11,12] We compared the effect of a number of pharmaco-logical inhibitors for various PKC isoforms on arsenite- and insulin-induced glucose uptake in 3T3-L1 adipocytes Ro

31-8220 inhibited insulin- and arsenite-induced glucose uptake with similar dose–response relations More precisely, an IC50 value of approximately 5 lMwas found for the inhibition

of insulin- and arsenite-induced glucose (Fig 7A) When PKC-k was purified by immunoprecipitation and subjected

to an in vitro kinase assay, a similar dose dependency for the inhibition of PKC-k (an IC50 of 5 lM) was observed (Fig 7B) Co-incubation with 50 lMof a peptide resembling the PKC-k pseudosubstrate domain reduced32P incorpor-ation by 90%, demonstrating the specificity of the assay In support of the data presented in Fig 3D, arsenite did not induce PKC-k activation over basal levels Hence, arsenite appears to require basal levels of PKC-k in conjunction with other signals to induce glucose uptake

In addition the PKC-inhibitors, chelerythrine chloride,

Ro 32-0432, bisindolylmaleimide I (BIM I) and Go¨ 6976 were studied at concentrations well above the IC50values for their respective conventional and novel PKC target proteins (Table 1) All inhibitors reduced TPA-induced ERK phosphorylation in 3T3-L1 adipocytes, demonstra-ting their functional interference with PKC (Fig 7C) Their effects on arsenite- and insulin-induced glucose uptake were minimal (Fig 7D) (although BIM I had a small but significant inhibitory effect), demonstrating that neither conventional nor novel PKC isoforms are involved in arsenite- or insulin-induced glucose uptake

The effect of myristoylated PKC-k/-f and PKC-a/-b pseudosubstrate peptides on arsenite-induced glucose uptake

To substantiate the observations made using Ro 31-8220 we investigated the effect of myristoylated peptide-inhibitors for PKC [11] on insulin- and arsenite-induced glucose uptake As can be seen in Fig 8B, a myristoylated peptide with a sequence similar to the pseudosubstrate domain of the atypical PKCs was capable of inhibiting insulin- as well

as arsenite-induced glucose uptake A peptide resembling the pseudosubstrate domain of conventional PKC-a/-b had

no significant inhibitory effect on either insulin- or arsenite induced glucose uptake (Fig 8B), whereas it did block TPA induced ERK phosphorylation demonstrating its functionality (Fig 8A) These observations corroborate the observations made with Ro 31-8220

Discussion

Insulin-induced glucose uptake by adipocytes is determined

by multiple factors, including: the translocation of glucose transporters from intracellular sites to the plasma mem-brane, expression levels of individual members of the glucose transporter family and by modulating the intrinsic activity (or, degree of occlusion) of glucose transporters (Fig 9)

Fig 5 The involvement of tyrosine kinase activity in arsenite-induced

glucose uptake 3T3-L1 adipocytes were pretreated with for 15 min

with 25 l M tyrphostin A25 as indicated Subsequently, adipocytes

were mock-treated (-), stimulated for 5 min with 100 n M insulin (INS)

or for 30 min with 0.5 m M arsenite (As) in the continued presence of

the pharmacological inhibitor (A) Total cell lysate (10 lg) was

sub-jected to immunoblot analysis using antibodies against phosphoY14 of

caveolin-1 (ap-Cav1), phosphotyrosine (ap-Tyr) (shown are the

IRS-bands at 180 kDa) and IRS-1 (aIRS) for equal loading (B) 3T3-L1

adipocytes treated as described above were immunoprecipitated using

antibodies against c-Cbl followed by immunoblot analysis using

antibodies against phosphotyrosine (ap-Tyr) or Cbl (ac-Cbl) (C)

3T3-L1 adipocytes were pretreated for 15 min with 25 l M tyrphostin A25.

Subsequently, adipocytes were mock-treated (basal), stimulated for

15 min with 100 n M insulin or for 30 min with 0.5 m M arsenite in the

continued presence of the pharmacological inhibitor and assayed for

2-DOGuptake Data are expressed as mean ± SEM of at least six

observations Statistically significant (*P < 0.05) when compared to

the samples not treated with tyrphostin Statistically significant

(P < 0.05) when compared to the basal (or arsenite) samples treated

with tyrphostin A25.

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Arsenite is a protein modifying agent known to react with

sulfhydryl groups in a discrete number of proteins As a

result these proteins are modified in their function and this

can couple back to altered activity of signal transduction

pathways

In this report we demonstrate that arsenite displays

insulin-mimicking effects in 3T3-L1 adipocytes: thus,

arse-nite stimulates 2-DOGuptake and induces translocation of

the insulin-responsive GLUT4 glucose transporter from the

low-density microsomal fraction towards the plasma

mem-brane Comparable to other stress-inducing agents [38,39]

arsenite acutely blocks insulin-induced glucose uptake

(Fig 1C), however, and in contrast to oxidative and

osmotic stress, arsenite did not interfere with early events

in insulin-induced signalling A normal level of

phosphory-lation of IRS-1,2 and PKB was observed by

insulin-induction after incubation with arsenite (data not shown)

Whereas PI-3¢ kinase activity is pivotal for

insulin-induced GLUT4 translocation, arsenite increases the uptake

of 2-DOGwithout the need for PI-3¢ kinase activity as

judged from the absence of an effect of arsenite on

PI-3¢ kinase activation and the lack of inhibition by either

wortmannin or LY 294002 Furthermore, arsenite does not

activate other signalling steps normally activated in response

to insulin, such as IR tyrosine kinase, IRS-1 and IRS-2

tyrosine phosphorylation, phosphorylation of PKC-k on T403 or phosphorylation of PKB on either Ser473 or Thr308 These observations suggest that the target of arsenite action resides downstream of PI-3¢ kinase or in a separate pathway

A PI-3¢ kinase-independent pathway in insulin-induced GLUT4 translocation has recently been identified and involves tyrosine phosphorylation on several residues of the proto-oncogene c-Cbl [13,40] and caveolin-1 [41] by the activated insulin receptor Arsenite also induces c-Cbl and caveolin-1 tyrosine phosphorylation in 3T3-L1 adipo-cytes, however, given that arsenite does not activate the insulin receptor (Fig 3A) the two processes are mechan-istically different The distinct nature of the insulin- and arsenite-induced tyrosine kinase activities is illustrated by the effects of tyrphostin A25 Whereas insulin-induced tyrosine kinase activity was attenuated (and Cbl-tyrosine phosphorylation levels even potentiated), all arsenite-induced tyrosine phosphorylation was strongly reduced The effects of tyrphostin A25 on insulin- and arsenite-induced glucose uptake mirrored these observations, i.e., insulin-induced glucose uptake was attenuated whereas arsenite-induced glucose uptake was lost These data also demonstrate that a tyrosine kinase activity is apparently required for the induction of glucose uptake by arsenite,

Fig 6 The effect of the p38 MAP kinase inhibitor, SB203580, on arsenite-induced glucose uptake and translocation of GLUT4 3T3-L1 adipocytes were pretreated for 30 min with 10 l M SB203580 (A–D) Subsequently adipocytes were mock-treated (basal) or stimulated as indicated with

100 n M insulin for 15 min (insulin) or with 0.5 m M arsenite for 30 min (arsenite) in the continued presence of the pharmacological inhibitor and assayed for 2-DOGuptake (A) Data are expressed as the mean value ± SEM of at least six observations Statistically significant (*P < 0.05) when compared to samples without SB203580 (B) 3T3-L1 adipocytes were lysed and subjected to immunoblot analysis using antibodies against p38 MAPK (p38), phospho-specific antibodies against p38 (p-p38) and MAPKAP-K2 (p-MAPKAP-K2) (C) 3T3-L1 adipocytes treated as described above were subjected to cell fractionation and the effect of SB203580 on GLUT4 translocation was determined by immunoblotting followed by quantification in a lumni-imager as described for Fig 2B Samples pretreated with SB203580 are indicated with SB Data are expressed as the mean ± SEM of three independent experiments (D) Representative immunoblot probed with anti-GLUT4 Igs, used to obtain the data described in C.

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as is the case for insulin The identity of the

tyrosine-kinase activity activated in response to arsenite remains to

be resolved

The pharmacological p38 MAPK inhibitor, SB203580,

affects insulin-induced glucose transport by affecting

intrinsic GLUT4 activity [35,36] Our results with this

inhibitor confirmed this observation Furthermore, we

demonstrate a similar effect on arsenite-induced glucose

uptake Pre-treatment with 10 lM SB203580 had no

effect on GLUT4 (or GLUT1) translocation but did

reduce arsenite-induced glucose uptake by 30% Thus,

our data show a similar contribution of p38-MAPK

activity in combination with GLUT4 translocation in

insulin- and arsenite-induced glucose uptake at the level

of modulating the GLUT4 mediated transport activity

Though we cannot fully exclude a similar effect of

SB203580 on GLUT1 as well, this seems unlikely given

that SB203850 had no effect whatsoever on arsenite- or

insulin-induced glucose uptake levels in 3T3-L1

preadipo-cytes (expressing GLUT1 and no GLUT4) (data not

shown)

The term coined for the modulatory effect of SB203850

is Ôintrinsic activityÕ [35], possibly by altering the speed of transition between ÔoutwardÕ and ÔinwardÕ conformations

of the transporter [42] The term ÔocclusionÕ has been used

to describe a state in which the GLUT4 transporter is fully inserted to the plasma membrane, but incapable of binding and/or transporting glucose yet [43] This could

be due to associating proteins blocking glucose transport, differences in LDM-derived and PM-membrane compo-sition and/or a conformational change in the GLUT4-transporter that is required for its activation If SB203580 hampers the progress through these stages, similar consequences are expected (i.e., GLUT4 being present

in the plasma membrane, but less glucose being taken up) Arsenite-induced glucose uptake, which demonstrates

a similar sensitivity to SB203580, may provide an additional tool for future research addressing these models

Cellular stresses like hypoxia [44] and hyperosmolarity [45] increase glucose uptake through an upregulation of the amount of GLUT1 Arsenite in contrast, does not increase

Fig 7 The effect of PKC-inhibitors on arsenite-induced glucose uptake 3T3-L1 adipocytes were incubated with the indicated concentrations of

Ro 31-8220 for 30 min prior to stimulation Subsequently, adipocytes were mock-treated (basal), stimulated with 100 n M insulin for 15 min (insulin) or 0.5 m M arsenite for 30 min (arsenite) in the continued presence of Ro 31-8220 (A) 2-DOGuptake was assayed and data are expressed

as mean ± SEM of two independent experiments each performed in triplicate (B) In vitro kinase assay performed in the continued presence of

Ro 31-8220 Incorporated counts (in k c.p.m.) are expressed as mean ± SEM of two independent experiments each performed in duplicate (C,D) 3T3-L1 adipocytes were pretreated for 30 min with 0.1 l M Go¨ 6976, 5 l M bisindolylmaleimide I (BIM I), 10 l M chelerythrine chloride (Chel-erythrine), or 10 l M Ro 32–0432 as indicated Subsequently, 3T3-L1 adipocytes were stimulated with 100 n M TPA for 15 min and analysed for ERK-1/2 phosphorylation (C) 2-DOGuptake was tested in a separate experiment (D) After pretreatment with the indicated pharmacological inhibitors, adipocytes were mock-treated (basal), stimulated with 100 n M insulin for 15 min (insulin), or 0.5 m M arsenite for 30 min (arsenite) in the continued presence of the inhibitors 2-DOGuptake was assayed and data are expressed as mean ± SEM of at least two independent experiments each performed in triplicate, statistically significant compared to the uninhibited samples (*P < 0.05).

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the amount of GLUT1 Indeed, treatment of the adipocytes

with the protein synthesis inhibitors cycloheximide or

emetine had no effect on arsenite-induced glucose uptake

(data not shown) Furthermore, the time-course of

arsenite-induced glucose uptake, being maximal after 30 min and

declining thereafter (Fig 1B) already seems to argue against

de novo synthesis of GLUT-transporters in mediating

arsenite-induced glucose uptake

Although most GLUT1 is already localized in the plasma

membrane of an unstimulated adipocyte [46], some GLUT1

is known to cotranslocate with GLUT4 [47] and Fig 2

C,D,E Moreover, treatment of 3T3-L1 adipocytes with

TPA induced the specific translocation of GLUT1 and not

GLUT4 towards the plasma membrane of 3T3-L1

adipo-cytes [48] Arsenite in contrast, induces the translocation of

GLUT1 at about half the levels obtained with insulin

Though failing to reach statistical significance (Fig 2D) this

effect was consistently reproducible (e.g Fig 2C,E) Thus,

clearly, arsenite differs from other types of cellular stress in

that it projects towards a more insulin-like response (i.e.,

translocation of GLUT1 and 4) albeit at a lower level of

efficiency

When applying multiple pharmacological- and

peptide-inhibitors for several PKC isoforms we observed a common

pattern of inhibition for insulin- and arsenite-induced

glucose uptake and similar concentration dependencies for the various agents Most notably, Ro 31-8220 inhibits both insulin- and arsenite-induced glucose uptake with an IC50of

5 lMsuggesting an involvement of atypical PKCs The IC50

of atypical PKC for BIM I is 5.8 lM, hence the significant reduction in glucose uptake measured using 5 lM(Fig 7D) fits with the observations made with Ro 31-8220 Inhibitors against conventional or novel PKCs such as Go¨ 6976, chelerythrine chloride and Ro 32-0432 (a compound struc-turally related to Ro 31-8220) (Table 1) remained without effect, or acted even in a slightly potentiating manner Furthermore, both insulin- and arsenite induced glucose uptake was inhibited by treatment with a myristoylated PKC-k/f pseudosubstrate peptide, but not significantly sensitive to treatment with a PKC-a/b pseudosubstrate A formal exclusion of other intracellular targets with similar sensitivities to the inhibitors mentioned cannot, however, be excluded

In the case of arsenite-induced glucose uptake, the myristoylated PKC-k/f pseudosubstrate peptide inhibited this response by approximately 50% (Fig 8B) Remark-ably, when the effect of Ro 31-8220 on arsenite-induced GLUT4 translocation was determined a similar reduction in GLUT4 translocation was observed (data not shown) This

is in contrast to the situation in response to insulin, where the inhibition is complete

Another observation was that in contrast to insulin, arsenite did not induce T-loop phosphorylation of PKC-k (Fig 3D), nor did we observe an increase in the amount of incorporated radiolabelled phosphate in immunoprecipi-tated PKC-k (data not shown) Indeed, when analysing PKC-k activity in an in vitro kinase assay, no induction of PKC-k activity in response to arsenite was observed (Fig 7B) Thus, taken together, these data suggest that arsenite does not activate PKC-k, but does require the basal

Fig 8 Arsenite-induced glucose uptake is inhibited by a myristoylated

PKC-k/-f, but not by PKC-a/-b pseudosubstrate peptide 3T3-L1

adipocytes were incubated with either myristoylated PKC-a/-b

pseudosubstrate (myrPKC-a/b ps), or myristoylated PKC-k/–f

pseudosubstrate (myrPKC-k/f ps) at the indicated concentrations for

1 h prior to stimulation (A) 3T3-L1 adipocytes were treated with

100 n M TPA for 15 min and subjected to immunoblotting as described

in the legend of Fig 7C (B) 2-DOGuptake was tested in a separate

experiment 3T3-L1 adipocytes were mock-treated (basal), stimulated

for 15 min with 100 n M insulin (insulin) or for 30 min with 0.5 m M

arsenite (arsenite) Data are expressed as mean ± SEM of at least two

independent experiments each performed in triplicate, statistically

significant compared to the uninhibited samples (*P < 0.05).

Fig 9 A model highlighting the insulin- and arsenite-induced pathways

to glucose uptake in 3T3-L1 adipocytes Our data suggest some com-mon steps in both arsenite- and insulin-induced glucose uptake: acti-vation of p38 MAPK and tyrosine-phosphorylation of c-Cbl In contrast to insulin, arsenite does not activate PI-3¢ kinase (and con-sequently does not activate PKC-k) However, the data suggests that basal levels of PKC-k activity are needed for arsenite-induced glucose uptake, as is indicated by the dashed arrow.

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