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Results In an effort to identify novel proteins that are part of the vegetal RNA localization machinery in Xenopus oocytes, tandem affinity purification TAP-tagged ver-sions of the known v

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machinery in Xenopus laevis oocytes

Jana Loeber1, Maike Claußen1, Olaf Jahn2and Tomas Pieler1

1 Department of Developmental Biochemistry, Go¨ttingen Center for Molecular Biosciences, University of Go¨ttingen, Germany

2 Proteomics Group, Max-Planck-Institute of Experimental Medicine, Go¨ttingen, Germany

Keywords

EF1a; RNA localization; 42Sp50; Vg1RBP;

Xenopus laevis oocytes

Correspondence

T Pieler, Department of Developmental

Biochemistry, Go¨ttingen Center for

Molecular Biosciences, University of

Go¨ttingen, Justus-von-Liebig-Weg 11,

37077 Go¨ttingen, Germany

Fax: +49 551 3914614

Tel: +49 551 395683

E-mail: tpieler@gwdg.de

(Received 28 February 2010, revised 30

August 2010, accepted 9 September 2010)

doi:10.1111/j.1742-4658.2010.07878.x

Localization of a specific subset of maternal mRNAs to the vegetal cortex of Xenopusoocytes is important for the regulation of germ layer formation and germ cell development It is driven by vegetal localization complexes that are formed with the corresponding signal sequences in the untranslated regions

of the mRNAs and with a number of different so-called localization proteins

In the context of the present study, we incorporated tagged variants of the known localization protein Vg1RBP into vegetal localization complexes by means of oocyte microinjection Immunoprecipitation of the corresponding RNPs allowed for the identification of novel Vg1RBP-associated proteins, such as the embryonic poly(A) binding protein, the Y-box RNA-packaging protein 2B and the oocyte-specific version of the elongation factor 1a (42Sp50) Incorporation of 42Sp50 into localization RNPs could be con-firmed by co-immunoprecipitation of Vg1RBP and Staufen1 with myc-tagged 42Sp50 Furthermore, myc-42Sp50 was found to co-sediment with the same two proteins in large, RNAse-sensitive complexes, as well as to associ-ate specifically with several vegetally localizing mRNAs but not with nonlo-calized control RNAs Finally, oocyte microinjection experiments reveal that 42Sp50 is a protein that shuttles between the nucleus and cytoplasm Taken together, these observations provide evidence for a novel function of 42Sp50

in the context of vegetal mRNA transport in Xenopus oocytes

Structured digital abstract

l MINT-7994313 : epab (uniprotkb: Q98SP8 ) physically interacts ( MI:0915 ) with Vg1RBP (uni-protkb: O73932 ) by anti tag coimmunoprecipitation ( MI:0007 )

l MINT-7994335 : 42Sp50 (uniprotkb: P17506 ) physically interacts ( MI:0915 ) with Vg1RBP (uniprotkb: O73932 ) by anti tag coimmunoprecipitation ( MI:0007 )

l MINT-7994166 : Vg1RBP (uniprotkb: O73932 ) physically interacts ( MI:0914 ) with Vg1RBP (uniprotkb: O73932 ), 42Sp50 (uniprotkb: P17506 ), frgy2-b (uniprotkb: P45441 ) and epab (uni-protkb: Q98SP8 ) by tandem affinity purification( MI:0676 )

l MINT-7994324 : frgy2-b (uniprotkb: P45441 ) physically interacts ( MI:0915 ) with Vg1RBP (uniprotkb: O73932 ) by anti tag coimmunoprecipitation ( MI:0007 )

l MINT-7994345 : 42Sp50 (uniprotkb: P17506 ) physically interacts ( MI:0914 ) with staufen (uniprotkb: Q5MNU4 ) and Vg1RBP (uniprotkb: O73932 ) by anti tag coimmunoprecipitation ( MI:0007 )

l MINT-7994363 : 42Sp50 (uniprotkb: P17506 ), Vg1RBP (uniprotkb: O73932 ), staufen (uniprotkb: Q5MNU4 ) and 40LoVe (uniprotkb: Q6GM69 ) colocalize ( MI:0403 ) by cosedimentation through density gradient ( MI:0029 )

l MINT-7994241 : Vg1RBP (uniprotkb: O73932 ) physically interacts ( MI:0914 ) with elrB (uni-protkb: Q91903 ), ElrA (uniprotkb: Q1JQ73 ), hnRNPI (uniprotkb: Q9PTS5 ), 40LoVe (uni-protkb: Q6GM69 ), staufen (uniprotkb: Q5MNU4 ) andVg1RBP (uniprotkb: O73932 ) by tandem affinity purification ( MI:0676 )

Abbreviations

EF1A, elongation factor 1a; ePAB, embryonic poly(A) binding protein; FRGY-2B, Y-box RNA-packaging protein 2B; LE, localization element;

OE, oocyte equivalent; TAP, tandem affinity purification; 42Sp50, oocyte-specific version of the elongation factor 1a.

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During oogenesis in Xenopus laevis, a group of

mater-nal transcripts becomes specifically localized to the

vegetal cortex By this means, an intracellular

asymme-try is created for subsequent use during early

embryo-nic development The respective vegetal mRNAs are

transported via two distinct routes [1] The early

(METRO-) pathway is activated in stage I–II oocytes;

RNAs associate with the mitochondrial cloud (also

referred to as the Balbiani body), a large conglomerate

enriched in mitochondria, endoplasmic reticulum

mem-branes and RNPs, also containing the germ plasm

Together with the mitochondrial cloud, the prospective

vegetal RNAs then migrate towards the vegetal cortex,

where they become anchored during stage III [1] The

association between the Balbiani body and the

mRNAs is considered to be established via a

diffu-sion–entrapment mechanism [2] and does not appear

to depend on the presence of intact microtubules [1];

however, a recent study provides evidence for a

facili-tating activity exerted by kinesin II [3] By contrast,

the late localization pathway can be efficiently blocked

when oocytes are treated with nocodazole, a

microtu-bule-depolymerizing drug [4] Although the late

locali-zing RNAs are excluded from the mitochondrial cloud

at the beginning of oogenesis, they accumulate between

the nucleus and vegetal pole during stage III and

sub-sequently translocate vegetally In stage IV oocytes,

the respective RNAs are found anchored at the cortex

of the entire vegetal hemisphere

All vegetally localizing RNAs contain regulatory

sequence elements in their untranslated regions, which

are necessary and sufficient for transport, and are

referred to as localization elements (LEs) In some

mRNAs, such as Vg1 or VegT, the number and

rela-tive positioning of short consensus sequence motifs

determines the localization efficiency [5–7] However,

the LEs of other localizing mRNAs, such as fatvg,

Xdead end, Xvelo1 and Xwnt11, contain only few or

none of these motifs, although they are still capable of

mediating vegetal transport [8–11] Therefore, the

sec-ondary structure of the LEs may as well be critical for

RNA localization, as is the case in Drosophila and

yeast [12–14]

LEs recruit trans-acting proteins, such as Vg1RBP,

hnRNPI⁄ PTB, Prrp, Staufen, 40LoVe and ElrA ⁄ B,

thereby forming the so-called localization complex or

‘locasome’ [5,15–20] Discrete RNP assembly steps

have been defined for Vg1 mRNA in the context of

the late vegetal RNA transport pathway In the

nucleus, Vg1 is recognized by the RNA-binding

pro-teins Vg1RBP and hnRNP I [7,21]; the export of this

complex into the cytoplasm is followed by a structural reorganization of the RNP Although, in the nucleus, the association between Vg1RBP and hnRNPI does not depend on the presence of RNA, the same interac-tion becomes RNA-dependent in the cytoplasm [21] Moreover, other proteins such as Staufen1 and Prrp join the complex in the cytoplasm [16–18] The trans-acting factors ElrA and 40LoVe can be detected in the nucleus as well as in the cytoplasm [20,22] However, it

is not yet clear at what stage of the transport process they join the localization complex Interestingly, Stau-fen has been found to interact with kinesin in X laevis oocytes, and might therefore provide the link between the localizing particle and a motor protein [18] The mature RNP eventually migrates to the vegetal cortex most likely along microtubules in a plus-end directed transport as the cargo of a kinesin motor [4,18,23,24]

At the vegetal cortex, the RNA molecule becomes anchored Cortical anchoring depends not only on the cytoskeletal network, but also on the presence of other localizing RNAs, such as Xlsirts and VegT [1,19,25] Although the RNP is assumed to dissociate at the cor-tex, trans-acting factors such as Prrp, ElrA, Staufen and 40LoVe remain enriched at the vegetal pole

in stage VI oocytes, when localization is finished [16,18–20]

To identify novel protein components of vegetal transport particles, we used over-expression of a tagged version of Vg1RBP to fish for novel binding partners that might play a role in RNA localization

We identified an oocyte-specific isoform of the protein translation elongation factor 1a (EF1A) as a novel Vg1RBP-interacting protein that is a specific compo-nent of vegetally localizing RNPs in Xenopus oocytes

Results

In an effort to identify novel proteins that are part of the vegetal RNA localization machinery in Xenopus oocytes, tandem affinity purification (TAP)-tagged ver-sions of the known vegetal localization factor Vg1RBP were expressed in stage III and IV X laevis oocytes by means of mRNA microinjection Two different tagged versions of Vg1RBP were employed: one carrying the TAP-tag at the N-terminus (N-TAP-Vg1RBP), and another one carrying it at the C-terminus (C-TAP-Vg1RBP) Lysates from microinjected oocytes were incubated with IgG sepharose beads and immobilized protein complexes containing TAP-Vg1RBP were eluted by proteolytic cleavage of Vg1RBP from the protein A moiety under native conditions; a control

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lysate from oocytes expressing the TAP-tag only

(TAP) was included Proteins contained in these

pre-parations were separated by SDS⁄ PAGE and

visua-lized by colloidal Coomassie staining (Fig 1A); the

arrays of proteins interacting with either

N-TAP-Vg1RBP or C-TAP-N-TAP-Vg1RBP were indistinguishable

from each other Proteins specifically interacting with

Vg1RBP were isolated and subjected to MS protein

identification Several of the protein species identified

by this means correspond to CBP-Vg1RBP (containing

the calmodulin binding peptide of the TAP-tag) or

endogenous Vg1RBP, as expected because of its

known ability to form homodimers, or degradation

products of the same protein Three novel proteins

could be identified that specifically co-purify with

Vg1RBP: embryonic poly(A)-binding protein (ePAB;

NCBI accession number: gi|13540314), Y-box protein

2B (FRGY-2B; NCBI accession number: gi|1175534)

and an oocyte-specific version of EF1A (42Sp50;

NCBI accession number: gi|416929)

The fact that other known localization factors, such

as Staufen or hnRNPI, were not identified, does not

necessarily imply that these proteins were not present

in the protein complex analyzed in the present study;

only proteins strongly stained by Coomassie were

reliably identified by MS analysis Different stoichio-metries of individual protein components, which assemble into one RNP with Vg1RBP, as well as struc-tural heterogeneity of RNPs containing Vg1RBP, may account for the fact that the expected interaction part-ners for Vg1RBP were not detected by Coomassie staining and MS analysis To confirm the presence of known localization factors, we analyzed TAP-Vg1RBP pulldown eluate by western blotting (Fig 1B) Staufen, 40LoVe, hnRNPI, ElrA and ElrB were found to co-purify with TAP-Vg1RBP, whereas GAPDH could not be detected This indicates that localization com-plexes were indeed isolated using the approach employed in the present study

The association between the novel proteins identified and Vg1RBP was verified by reverse co-immunoprecipi-tation For this purpose, Xenopus oocytes were micro-injected with synthetic mRNAs encoding myc-tagged versions of ePAB (myc-ePAB), FRGY-2B (myc-FRGY) and 42Sp50 (myc-42Sp50); complexes forming with these proteins were immunoprecipitated with a myc-specific antibody and co-precipitating Vg1RBP detected

by western blotting (Fig 2) It was found that endo-genous Vg1RBP is efficiently co-precipitated with ePAB

as well as FRGY-2B, and specifically, although with

Fig 1 Identification of Vg1RBP-interacting proteins (A) Oocyte extract prepared from uninjected stage III–IV oocytes and stage III–IV oocytes expressing either a TAP tag alone, N-terminally (N-TAP) or C-terminally (C-TAP) TAP-tagged Vg1RBP was incubated with IgG-sephar-ose beads and eluted by TEV protease cleavage of the TAP tag Eluted proteins were separated on 10% SDS ⁄ PAGE and visualized by colloi-dal Coomassie staining M, protein size marker The bands marked by blue lines were excised and analyzed by MS Putative Vg1RBP binding partners identified are ePAB, FRGY-2B and 42Sp50 Degradation products of Vg1RBP are marked with an asterisk (*) and proteins that could not be identified are labelled as n.i (B) Lysate from uninjected oocytes and oocytes expressing TAP or N-terminally TAP-tagged Vg1RBP was processed as above and analyzed by western blotting for the presence of known localization factors Input corresponds to 1%

of the material used in the pulldown experiment The presence of the TAP-Vg1RBP band in the anti-Staufen blot is a result of the strong binding of secondary anti-rabbit serum to the protein-A moiety of the TAP-tag Anti-CBP serum was used to show the expression of the TAP-tag alone.

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reduced efficiency, also with 42Sp50 These differences

in yield could reflect different protein stoichiometries in

the complexes that form After RNase-digestion,

Vg1RBP could no longer be detected in the

immunopre-cipitate, indicating that the interactions of these

differ-ent proteins are likely to be indirect, depending on the

presence of intact RNA as integral component of the

RNP

Association of 42Sp50 with mRNA has not been

reported previously If 42Sp50 is involved in vegetal

mRNA localization in Xenopus oocytes, as suggested

by its association with Vg1RBP, it would be expected

also to interact with other trans-acting localization

fac-tors, such as Staufen1 Co-immunoprecipitation

experi-ments from myc-42Sp50 programmed oocyte extract

do indeed reveal an RNA-dependent association of

42Sp50 with Staufen1 in addition to Vg1RBP (Fig 3)

Additional evidence for these proteins constituting

one RNP comes from density gradient centrifugation

analysis; fractionation of S16 total lysate from stage

III⁄ IV oocytes on a 5–60% glycerol gradient, followed

by western blotting, reveals 42Sp50 enrichment in high

density fractions together with Staufen1 and Vg1RBP

(Fig 4) These high density fractions contain large RNPs, with a size similar to 80S ribosomes; sensitivity

to RNAse treatment indicates that the RNA serves as

a scaffold for protein binding rather than protein–pro-tein interactions providing the driving force for the formation of these very large assemblies 42S tRNA storage particles that contain 42Sp50 do not co-migrate with 80S ribosomes and they are specific to stage I⁄ II oocytes [26] Taken together, these experi-mental observations provide strong evidence for 42Sp50 as being part of one large RNP complex together with other proteins known to serve functions

in vegetal RNA localization in Xenopus oocytes

If 42Sp50 was a trans-acting localization factor, it should be specifically associated with known vegetally localizing mRNA molecules To determine whether endogenous oocyte mRNAs are in a complex with

Fig 2 Vg1RBP interacts with ePAB, FRGY-2B and 42Sp50 in an RNase-dependent manner Stage III–IV oocytes were injected with RNA encoding either myc-tagged ePAB, FRGY or 42Sp50 Oocyte extract was prepared and subjected to immunoprecipitation with anti-myc serum in the presence or absence of RNase The precipitate was analyzed by SDS ⁄ PAGE and western blotting for the presence of Vg1RBP.

In a control immunoprecipitation with extract from uninjected oocytes, no Vg1RBP could be detected As input, 1% (for analysis with anti-Vg1RBP serum) or 20% (for analysis with anti-myc serum) of the total oocyte extract was loaded.

Fig 3 42Sp50 associates with Staufen1 in an RNase-dependent

manner Stage III oocytes were injected with Cap-RNA encoding

myc-42Sp50 and incubated overnight to allow protein expression.

Oocyte extract was used for co-immunoprecipitation using anti-myc

serum Precipitated proteins were analyzed by SDS ⁄ PAGE and

western blotting 42Sp50 interacts with both Vg1RBP and Staufen1

in the presence of intact RNA but not if cellular RNA is destroyed

by RNase digestion.

Fig 4 42Sp50 co-migrates with known components of the locali-zation complex in a glycerol gradient Extract from stage III–IV oocytes expressing myc-42Sp50 was fractionated on a 5–60% glycerol gradient either in the presence or absence of RNase Eleven fractions were collected and split into two aliquots to allow the detection of several proteins from the same gradient The fractions were subjected to SDS ⁄ PAGE, and western blot analyses were performed using specific antibodies against Vg1RBP, Staufen1 and 40LoVe or anti-myc serum to detect myc-42Sp50 Fractions 7–9 are enriched in the known localization factors Vg1RBP and Staufen1, and are therefore labelled as locasome.

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42Sp50, we performed RNA co-immunoprecipitaion

experiments For this purpose, synthetic mRNA

encoding myc-tagged 42Sp50 was microinjected into

stage III and IV oocytes; S16 lysate was prepared after

24 h of incubation and used for an

immunoprecipita-tion with anti-myc The RNA was eluted from the

immunopellet and characterized for the presence of

dif-ferent mRNAs by quantitative real-time RT-PCR

cor-rected for the abundance of individual mRNA species

[20] It was found that of the three vegetally localizing

mRNAs tested, two, namely VegT and XNIF, are

sig-nificantly enriched in RNPs with 42Sp50 The

distribu-tion of only one of the vegetally enriched mRNAs,

namely Vg1, is similar to the nonlocalizing mRNAs

ornithine decarboxylase and lamin B1 (Fig 5) A

simi-lar result was obtained for RNP immunoprecipitation

with myc-tagged Vg1RBP (data not shown)

RNPs destined for vegetal localization assemble in

the oocyte nucleus and undergo at least one

remodel-ling step after export into the cytoplasm [7,21];

Vg1RBP has been shown to be part of the nuclear as

well as of the cytoplasmic vegetal-transport-RNP,

whereas Staufen1 joins the complex only in the

cyto-plasm [21] By means of immunolocalization on oocyte

sections, 42Sp50 was mainly detected in the cytoplasm

of stage I⁄ II oocytes [27,28] When nuclear and

cytoplasmic lysate from manually dissected stage III

oocytes were analyzed for the presence of myc-tagged

42Sp50 expressed by means of mRNA microinjection (Fig 6A), it was found that the majority of the protein

is similarly detected in the cytoplasmic fraction; how-ever, a small but perhaps significant amount of 42Sp50

is found in the nucleus The same blot was also probed with specific antibodies against Staufen1 and Vg1RBP;

as expected, Staufen1 was almost exclusively detected

in the cytoplasm; this was also the case for Vg1RBP The presence of 42Sp50 in nucleus and cytoplasm indicates that it might be a shuttling protein with a function in the nuclear export of localizing mRNAs

To determine whether 42Sp50 is capable of shuttling,

we injected the radioactively labelled in vitro-translated protein either into the nucleus or into the cytoplasm of

X laevis oocytes, isolated the nuclei manually at differ-ent time points after injection, and analyzed the nuclear and cytoplasmic fractions by SDS⁄ PAGE and phosphoimaging (Fig 6B) Although a minor fraction

of 42Sp50 is exported from the nucleus after 3 and 5 h (lanes 12 and 14), no import into the nucleus could be seen, even after 5 h of incubation (lane 7) Because export but not import can be detected, the export rate appears to be much higher than the import rate This would be in line with the steady-state distribution of the protein as described above (Fig 6A)

Discussion

mRNA transport to the vegetal cortex of Xenopus oocytes occurs in the context of large RNPs that can incorporate tagged variants of known localization pro-teins such as Vg1RBP expressed by means of oocyte microinjection Immunoprecipitation of such RNPs allowed for the identification of novel Vg1RBP-asso-ciated proteins such as ePAB, FRGY-2B and 42Sp50 Incorporation of 42Sp50 into localization RNPs could

be confirmed by co-immunoprecipitation of Vg1RBP and Staufen1 with myc-tagged 42Sp50 Furthermore, myc-42Sp50 was found to co-sediment with the same two proteins in large, RNase-sensitive complexes, as well as to associate specifically with several vegetally localizing mRNAs but not with nonlocalized control RNAs Finally, oocyte microinjection experiments reveal that 42Sp50 is a protein that shuttles between nucleus and cytoplasm

ePAB, similar to the prototypical poly(A) binding protein, functions as a translational activator; however,

it is only expressed during Xenopus oogenesis and early embryogenesis [29,30] Interestingly, human prototypi-cal poly(A) binding protein, which is not only func-tionally, but also structurally closely related to ePAB, was reported to be in direct interaction with IMP1, similar to Vg1RBP, which is a member of the VICKZ

Fig 5 The 42Sp50 particle is specifically enriched in localizing

RNAs Extract from stage III–IV oocytes expressing myc-tagged

42Sp50 were subjected to immunoprecipitation using anti-myc

serum As a control, the same extract was used in a precipitation

without antibody Proteins and RNAs bound to the immunopellet

were eluted by incubation in 1% SDS RNA was isolated by

phenol ⁄ chloroform extraction Ten percent of the oocyte extract

was used for the isolation of total RNA using the same protocol.

RNA was reverse transcribed into cDNA and analyzed by

quantita-tive PCR Enrichment factors were calculated using the 2)DCT

method [47] as described in the Experimental procedures The

enrichment factor of each RNA was normalized to GAPDH, which

was set to one The mean of three independent experiments is

shown, with error bars indicating the standard deviation ODC,

ornithine decarboxylase.

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family of RNA binding proteins [31–33] Together with

the findings obtained in the present study, interaction

of VICKZ and poly(A) binding proteins thus appears

to define a conserved feature of mRNPs forming in

dif-ferent biological systems The function of these mRNPs

is obviously not solely related to RNA transport

FRGY-2B is a germ cell specific RNA packaging

protein that stabilizes stored mRNAs and prevents

their translation [34,35] Tanaka et al [36] have

identi-fied proteins associated with FRGY2 in Xenopus

oocytes Interestingly, and in full agreement with data

reported in the present study, both Vg1RBP and ePAB

were among the proteins identified It is not known

why proteins that function as translational repressors,

such as FRGY2, or as translational activators, such as

ePAB, should be part of one and the same complex;

on the basis of the experimental results obtained in the

present study, we cannot exclude the possibility that

ePAB and FRGY2 are indeed part of different RNPs

together with Vg1RBP and⁄ or 42Sp50 Translational

repression would contribute to localized protein

expression after RNA localization has occured It is

not known whether the function of FRGY2 might be

dominant over the one exerted by ePAB and⁄ or how

translational repression would eventually be relieved

Although ePAB and FRGY-2B thus appear to

inter-act with a broad spectrum of mRNAs, 42Sp50 was

ori-ginally identified as one of two proteins that are found

in association with tRNA molecules in the 42S storage particles 42Sp50 is specifically expressed in previtello-genic phases of oogenesis (stage I and II); in structure, the protein is closely related to EF1A and it also exhi-bits aminoacyl tRNA transfer activity [27,37] The finding that 42Sp50 is part of vegetal RNA localization complexes in Xenopus oocytes relates to the more recent demonstration that EF1A is required for the intracellular localization and cortical anchoring of b-actin mRNA in chicken embryonic fibroblasts [38]; furthermore, EF1A was reported previously to interact with components of the cytoskeleton such as actin [39]

On the basis of these observations, it was therefore proposed that the EF1A-actin complex serves as a scaffold for b-actin mRNA anchoring [38] A similar notion might hold true for 42Sp50 in the context of vegetal mRNA localization in Xenopus oocytes; because we classified 42Sp50 as a shuttling protein, it might join the localization complex in the nucleus and mediate anchoring to cortical actin upon arrival of the RNP at the vegetal pole of the oocyte In the context

of these localizing RNPs, but also as integral part of the 42S storage particle, 42Sp50 might exert an addi-tional function for RNA export from the nucleus; however, direct experimental evidence in support of such a notion is currently not available

A

B

Fig 6 Intracellular localization of 42Sp50 in X laevis oocytes (A) 42Sp50 is present in the cytoplasm and in the nucleus The nuclei from stage III oocytes expressing myc-42Sp50 were manually isolated Nuclear (1–10 OE) and cytoplasmic fractions (0.5 and 1 OE) were analyzed

by SDS⁄ PAGE and western blotting using anti-myc serum As a control, the membrane was probed with anti-Vg1RBP and anti-Staufen1 sera Approximately 5% of myc-42Sp50 can be detected in the nucleus, whereas endogenous Vg1RBP or Staufen is not visible in the nuclear fraction (B) 42Sp50 shuttles between nucleus and cytoplasm Myc-42Sp50 was expressed in vitro in rabbit reticulocyte lysate, and radiolabelled with [ 35 S]methionin The reticulocyte lysate was injected either into the nucleus or the cytoplasm of stage VI oocytes After incubation for 0, 3 and 5 h, respectively, the nuclei and cytoplasms of 15 oocytes per timepoint were manually separated Myc-42Sp50 was recovered from the cytoplasmic and nuclear fractions by immunoprecipitation using anti-myc serum, separated by SDS ⁄ PAGE and analyzed

by phosphoimaging As a positive control, ribosomal protein L5 was co-injected Although 42Sp50 is exported from the nucleus, nuclear import cannot be detected.

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Because 42Sp50 was originally identified as a tRNA

specific RNA-binding protein and the experiments

con-ducted in the present study had revealed that it is in a

large complex with several different vegetally localizing

mRNAs and localization proteins such as Staufen1

and Vg1RBP, we also tested for direct binding of

42Sp50 to the LEs of different vegetal mRNAs For

this purpose, lysate from stage III and IV oocytes

expressing myc-tagged 42Sp50 was employed for UV

crosslinking experiments; however, no direct

interac-tion of 42Sp50 with the different LEs could be

demon-strated (data not shown) These negative results

indicate that 42Sp50 is either not in direct contact with

the LEs or that it associates with a different region of

the corresponding mRNAs To address the function of

42Sp50 in the process of vegetal mRNA localization

more directly, we aimed to generate dominant negative

effects by microinjection of various deletion mutants

of 42Sp50 into stage III⁄ IV oocytes However, reporter

RNA localization was found not to be affected in

these experiments (data not shown); because another

assay for the putative dominant negative activity of

the 42Sp50 deletion constructs is unavailable, the

inter-pretation of these observations remains elusive

Experimental procedures

Plasmids

The expression plasmids used in the TAP technique

(pCS2+-N-TAP-Vg1RBP and pCS2+-C-TAP-Vg1RBP)

were generated by inserting the coding sequence of the

TAP tag derived from pZome-1-N or pZome-1-C

(Euro-scarf, Heidelberg, Germany) into the BamHI and EcoRI

sites of the pCS2+ plasmid The full length coding region

of Vg1RBP (allele D, obtained from J Yisraeli) [40] was

ligated into the EcoRI site of the resulting pCS+-N-TAP

and pCS2+-C-TAP vectors The full length coding regions

of Xenopus 42Sp50 and ePAB were cloned from EST clones

of the NIBB X laevis project into the EcoRI and XbaI

sites of pCS2+-MT [41] The full length coding region of

FRGY-2B was amplified from oocyte cDNA using the

primers FRGY-2B_F: 5¢-GGAATTCCATGAGTGAGGC

GGAACC-3¢ and FRGY-2B_R: 5¢-GGTCTAGACAGCG

ACTGAGTTCATTCTG-3¢ and ligated into the EcoRI and

XbaI sites of pCS2+-MT

Oocyte microinjection and cultivation

Oocytes were obtained surgically from X laevis females,

defolliculated in 2.5 mgÆmL)1 Blendzyme 3 (Roche,

Mannheim, Germany) and stages III–IV were sorted

according to size [42] Cap-RNA was prepared from

pCS2+-TAP-Vg1RBP or pCS2+-myc-42Sp50, which were linearized with NotI using the mMessage mMachine kit (Ambion, Austin, TX, USA) and purified using the RNeasy kit (Qiagen, Hilden, Germany) Oocytes were injected with

15 nL of RNA (250–500 ngÆlL)1) each and incubated in

1· NaCl ⁄ Mes (10 mm Hepes, pH 7.4), 88 mm NaCl, 1 mm KCl, 2.4 mm NaHCO3, 0.82 mm MgSO4, 0.41 mm CaCl2, 0.66 mm KNO3) at 18C for 20–24 h Oocytes were har-vested in batches of 100, shock-frozen in liquid nitrogen and stored at)80 C until further use

For import and export assays, stage VI oocytes were injected with radioactively-labelled proteins produced in reticulocyte lysate programmed with pCS2+-myc-42Sp50

or pCS2+myc-L5 [43] and incubated in 1· NaCl ⁄ Mes at

18C for up to 6 h After incubation, nuclei were manually isolated with forceps The red colour of the reticulocyte lysate served as an indicator for successful nuclear injection Nucleus and cytoplasm of 15 oocytes per time point were homogenized in 500 lL of NET-2 buffer (50 mm Tris⁄ HCl,

pH 7.4, 150 mm NaCl, 0.05% Nonidet P-40), supplemented with protease inhibitors (Roche) and incubated with pro-tein-G-sepharose coupled anti-myc sera for 1 h at room temperature The immunoprecipitates were washed three times with NET-2, separated by SDS⁄ PAGE and analyzed

by phosphoimaging

Oocyte extract preparation and immuno-precipitation

Oocytes were lysed in IPP145 buffer (50 mm Tris⁄ HCl, pH 8.0), 145 mm NaCl, 0.05% NP-40, 5% glycerol, 1 mm phe-nylmethanesulfonyl fluoride, Proteinase Inhibitors (Roche)

in diethylpyrocarbonate-treated water) at 5 lL per oocyte equivalent (OE) After centrifugation at 16 000 g, yolk pro-teins were removed from the supernatant (S16) by Freon extraction (DuPont, Wilmington, DE, USA) The extract

of 100 OE was incubated with 1 lL of anti-myc serum for 1–

2 h at 4C and precipitated with 15 lL Protein-A-sepharose (GE Healthcare, Milwaukee, WI, USA) for 1 h up to over-night at 4C If indicated, 5 lL of RNase A (10 mgÆmL)1) was added together with the antibody Immunopellets were washed with ice-cold IPP145, mixed with 30 lL of 2· SDS loading dye and analyzed by western blotting

IgG affinity chromatography For the large scale IgG pulldown, 1000 oocytes (approxi-mately 9 mg of total protein) were used The oocytes were lysed in 5 lL of IPP145 per OE and Freon-extracted S16 lysate was prepared Three hundred microlitres of IgG-sepharose was added and incubated at 4C overnight The IgG-pellet was then washed in ice-cold IPP145 and subsequently in TEV digestion buffer (50 mm Tris, pH 7.5,

50 mm NaCl, 0.1% NP40, 5% glycerol) The TEV digest

Trang 8

was performed in 6 mL of TEV digestion buffer using

150 U of AcTEV (Invitrogen, Karlsruhe, Germany) at

16C for 4 h To elute the proteins from the IgG beads,

the NaCl concentration was increased to 150 mm and the

mixture was incubated for another 2 h at 16C The

volume of the eluate was reduced by ultracentrifugation

through Vivaspin columns (Sartorius, Go¨ttingen,

Ger-many), the proteins were precipitated with trichloroethane,

and visualized on an 8–16% SDS gel by colloidal

Coomas-sie staining Protein bands were picked manually and

pro-cessed for MS protein identification For the western blot

analysis of the IgG purified complexes, 100 oocytes

expres-sing either TAP tag alone or TAP-Vg1RBP, as well as

uninjected oocytes, were used, in accordance with the

affi-nity purification protocol described above

SDS/PAGE, western blot analysis and colloidal

Coomassie staining

For western blot analysis, proteins were separated by 10%

SDS⁄ PAGE and electroblotted onto nitrocellulose

membrane Proteins were detected using antibodies against

myc-tag (9E10; Sigma, St Louis, MO, USA), Vg1RBP

[J Yisraeli (University of Cambridge, UK)], Staufen1

[N Standart (Hebrew University, Jerusalem, Israel)],

40LoVe [I Mattaj (EMBL, Heidelberg, Germany)],

anti-hnRNPI (4E11; Antibodies-online,

http://www.antibodies-online.com), HuR (Santa Cruz Biotechnology, Santa Cruz,

CA, USA), Calmodulin-binding peptide (Upstate

Biotech-nology, Lake Placid, NY, USA) and GAPDH (Abcam,

Cambridge, MA, USA)

For staining with colloidal Coomassie, the gel was fixed

in 10% acetic acid and 40% ethanol for 1 h, washed twice

in distilled water and incubated in freshly prepared staining

solution overnight The staining solution was prepared as a

stock containing 0.1% (w⁄ v) Coomassie Brilliant Blue

G250, 2% (w⁄ v) ortho-phosphoric acid and 10% (w ⁄ v)

ammonium sulfate Four parts of this stock were mixed

with one part methanol and used immediately

Identification of proteins by MS

Manually excised gel plugs were subjected to an automated

platform for the identification of gel-separated proteins

[44] as described in recent large-scale proteome studies

[45,46] An Ultraflex MALDI-TOF-mass spectrometer

(Bruker Daltonics, Bremen, Germany) was used to acquire

both peptide mass fingerprint and fragment ion spectra,

resulting in confident protein identifications based on

sequence information and peptide mass Database searches

in the NCBI nonredundant primary sequence database

restricted to the taxonomy X laevis were performed using

the mascot, version 2.0 (Matrix Science, Boston, MA,

USA) with the parameter settings described previously

[45,46] All datasets were researched without taxonomy

restriction to account for potential matches to sequences from Xenopus tropicalis The minimal requirement for accepting a protein as identified was at least one peptide sequence match above homology threshold in coincidence with at least four peptide masses assigned in the peptide mass fingerprint

Co-immunoprecipitation and RT-PCR analysis

In total, 200 myc-42Sp50 expressing stage III–IV oocytes were lysed in 800 lL of IPP145 S16 lysate was prepared Three hundred microlitres of S16 were used for immuno-precipitation with anti-myc serum As a control, the same amount S16 was processed in parallel without antibody Precipitated proteins and RNAs were eluted by short incu-bation in IPP145 containing 1% SDS and 5 lgÆmL)1 glyco-gen RNAs were isolated by phenol⁄ chloroform extraction and NH4+ acetate⁄ ethanol precipitation The RNA pellet was washed in 80% ethanol, dried and resuspended in

20 lL of diethylpyrocarbonate-treated water Thirty micro-litres of S16 were used for the isolation of total RNA employing the same protocol

In total, 1.5 lL of precipitated RNA or 0.3 lL (2%) of total RNA were reverse-transcribed in a 10 lL reaction Some 2.5 lL of cDNA were analyzed by quantitative PCR

in a 25 lL reaction using the iQ SYBR Green Supermix and the iCycler system (Bio-Rad, Munich, Germany) The primers used for the amplification have been described pre-viously [20]

To determine the specific enrichment of the RNAs ana-lyzed, the 2)DCTmethod [47] was used The enrichment factor

F was calculated as: F = E1· E2⁄ E3 (E1= 2)[CT (myc-IP) )

CT (total)]

, E2= 2)[CT (myc-IP) ) CT (control ) IP)], E3=

2)[CT (control ) IP) ) CT (total)]) as reported previously [20] The enrichment factor for each RNA was normalized to GAPDH, which was set to 1

Acknowledgements

The authors would like to thank J Yisraeli (Hebrew University, Jerusalem, Israel) for providing the a-Vg1RBP antibody; N Standart (University of Cambridge, UK) for providing the a-XStaufen 1 antibody; K Czaplinski and I W Mattaj (EMBL, Heidelberg, Germany) for providing the a-40LoVe antibody; and Andreas Nolte for help with the DNA sequencing This work was supported by funds from the Deutsche Forschungsgemeinschaft to T.P

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