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Tài liệu Báo cáo khoa học: Evidence for interactions between domains of TatA and TatB from mutagenesis of the TatABC subunits of the twin-arginine translocase docx

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Tiêu đề Evidence for interactions between domains of TatA and TatB from mutagenesis of the TatABC subunits of the twin-arginine translocase
Tác giả Claire M. L. Barrett, Colin Robinson
Trường học University of Warwick
Chuyên ngành Biological Sciences
Thể loại báo cáo khoa học
Năm xuất bản 2005
Thành phố Coventry
Định dạng
Số trang 15
Dung lượng 546,51 KB

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Near-complete restoration of activity in TatA mutants is achieved by the simultaneous presence of a V12P mutation in the TatB TM span, strongly implying a direct functional interaction b

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and TatB from mutagenesis of the TatABC subunits

of the twin-arginine translocase

Claire M L Barrett and Colin Robinson

Department of Biological Sciences, University of Warwick, Coventry, UK

The twin-arginine translocation (Tat) system operates

in the plasma membranes of a wide range of bacteria

as well as the thylakoid membrane in plant

chloro-plasts (reviewed in [1,2]) Working in parallel with the

Sec system, it is responsible for the export of a subset

of proteins into the periplasm, outer membrane or

extracellular medium, and the primary defining

attrib-ute of the system is its ability to transport proteins in

a fully folded state [3,4] Particular attention has

centred on a series of periplasmic proteins that are

exported only after binding redox cofactors such as

FeS or molybdopterin centres [5–8] although it should

also be emphasized that the system also transports proteins that do not bind cofactors [1,2]

Substrates for the Tat pathway are exported post-translationally [8] after synthesis with cleavable, N-ter-minal signal peptides that almost invariably contain an essential twin-arginine motif in the N-terminal domain [9,10] They then interact with a translocon in the inner membrane that consists, minimally, of three sub-units (TatABC) in Escherichia coli and several other Gram-negative bacteria studied to date Genetic stud-ies indicate that the tatABC genes are all important for Tat activity although a fourth gene, tatE, encodes

Keywords

green fluorescent protein (GFP); Tat system;

twin-arginine; protein transport; signal

peptide

Correspondence

C Robinson, Department of Biological

Sciences, University of Warwick, Coventry,

CV4 7AL, UK

Fax: +44 2476523701

Tel: +44 2476523557

E-mail: Crobinson@bio.warwick.ac.uk

(Received 13 December 2004, revised 25

February 2005, accepted 8 March 2005)

doi:10.1111/j.1742-4658.2005.04654.x

The twin-arginine translocation (Tat) system transports folded proteins across the bacterial plasma membrane Three subunits, TatA, B and C, are known to be involved but their modes of action are poorly understood, as are the inter-subunit interactions occurring within Tat complexes We have generated mutations in the single transmembrane (TM) spans of TatA and TatB, with the aim of generating structural distortions We show that sub-stitution in TatB of three residues by glycine, or a single residue by proline, has no detectable effect on translocation, whereas the presence of three gly-cines in the TatA TM span completely blocks Tat translocation activity The results show that the integrity of the TatA TM span is vital for Tat activity, whereas that of TatB can accommodate large-scale distortions Near-complete restoration of activity in TatA mutants is achieved by the simultaneous presence of a V12P mutation in the TatB TM span, strongly implying a direct functional interaction between the TatA⁄ B TM spans

We also analyzed the predicted amphipathic regions in TatA and TatB and again find evidence of direct interaction; benign mutations in either subunit completely blocked translocation of two Tat substrates when present in combination Finally, we have re-examined the effects of previously ana-lyzed TatABC mutations under conditions of high translocation activity Among numerous TatA or TatB mutations tested, TatA F39A alone blocked translocation, and only substitutions of P48 and F94 in TatC blocked translocation activity

Abbreviations

GFP, green fluorescent protein; Tat, twin-arginine translocation; TM, transmembrane; TMAO, trimethylamine N-oxide; TorA, TMAO

reductase.

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a TatA paralog of minor importance in some species

[7,8,11–13] Only two tat genes (designated tatC and

tatA) are thought to be important in some

Gram-positive species, with a single gene product apparently

fulfilling both TatA and TatB functions [14–16]

Studies on the Tat mechanism are at an early stage

The Tat subunits are not related to any proteins in the

database and most studies point to a mechanism that

is unique among known protein transport systems

However, recent studies have begun to unravel some

salient features of this system Protein expression⁄

puri-fication approaches have resulted in the

characteriza-tion of two distinct complexes in E coli: a TatABC

complex and homo-oligomeric TatA complex The

TatABC complex has a mass of  600 kDa in

deter-gent and contains multiple copies of TatABC; within

this complex, TatB and TatC are in stoichiometric

amounts and the two subunits appear to function as a

unit [17] Approximately equal numbers of TatA

sub-units are present [17,18] but the vast majority of TatA

is found as separate, apparently homo-oligomeric

com-plexes [17,19,20] In vitro cross-linking studies on the

plant thylakoid [21] or E coli Tat system [22] have

shown that substrates initially bind to the TatB and

TatC subunits, and it thus appears that these subunits

cooperate to form the substrate binding site In plants,

the TatA homolog was only found to cross-link to

the Hcf106⁄ cpTatC complex (corresponding to bacterial

TatBC) in the presence of substrate and a proton

motive force [23] On the basis of these studies, it has

been proposed that binding of substrate to the TatBC

subunits triggers the recruitment of the separate TatA

complex to form an active translocation system

In an effort to pinpoint important regions of the Tat

subunits, the three proteins have been subjected to

site-specific mutagenesis and a number of key regions

or residues have been identified [24–27] TatA and

TatB are single-span proteins with C-terminal,

cyto-plasmic domains and each has also been truncated

from the C-terminus in order to delineate the regions

important for activity [28] Site-specific mutagenesis

has also been used to assess the importance of residues

in the predicted amphipathic domains and cytoplasmic

regions of TatA and TatB, and the highly conserved

residues of TatC have also been probed [24–27] In this

report we have analyzed the transmembrane regions of

TatA and TatB, in an effort to analyze their

import-ance for Tat function We show that mutations

designed to destabilize the TatB TM span through

sub-stitution by proline or multiple glycine residues have

no detectable effect, whereas some of the TatA

mutants are severely affected or blocked in

transloca-tion activity We also present evidence for interactransloca-tions

between the TM spans of TatA and TatB, and between the amphipathic regions Finally, we have re-examined the numerous mutations made previously

in TatA, B and C and we present new information on potentially important TatA and TatC mutants

Results

Analysis of TatA and TatB mutants The overall structures of the TatA and TatB subunits are similar: both contain a single TM span, with very short periplasmic N-terminal regions and cytoplasmic domains that are relatively small in the case of TatA ( 40 residues) and larger in TatB ( 90 residues) The TM spans and cytoplasmic domains are separated

by regions that are strongly predicted to form amphi-pathic a-helices [19,20] In the present study we have generated mutations in the TM and amphipathic regions of TatA and TatB (see below) in order to probe the importance of this region, especially with respect to a possible role for TatA as the translocation channel In order to present a comprehensive analysis

we have analyzed in parallel the translocation activity

of TatABC mutants described in several previous stud-ies [24–27] This was considered important because one

of the mutants exhibited unexpected properties when compared with previous findings

The effects of the mutations were analyzed using two types of export assay The first involves expression

of the mutated tatABC operon in the arabinose-indu-cible pBAD24 vector in a tat null background (Dtat-ABCDE strain) The cells were fractionated and the distribution of a known Tat substrate, trimethylamine N-oxide (TMAO) reductase (TorA) was analysed using

a native gel activity assay This assay is not quantita-tive but defects in translocation are usually apparent through an increased accumulation of TorA in the cytoplasm It should be noted that this vector expres-ses the tatABC operon by a factor of  10–20 fold higher compared with wild-type TatABC levels This means that minor, and even moderate defects in trans-location activity may not be revealed because the higher levels of Tat apparatus might be able to com-pensate for defects Moreover, this assay is qualitative rather than quantitative because the appearance of the TorA signal in the native gels is not linear with time

In summary, this assay is best suited for identification

of major defects in translocation activity

The second assay involves synthesis of a construct comprising the presequence of TorA linked to green fluorescent protein (GFP), which is efficiently exported

by the Tat pathway under these conditions [24,26,28]

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In these experiments, synthesis of TorA-GFP was

induced for 2 h using the pBAD vector, after which

the arabinose was removed and IPTG was added to

induce expression of tatABC from the compatible

pEXT22 plasmid (although this plasmid is relatively

leaky, thus TatABC are synthesized at appreciable

rates throughout the growth of the cells) Membranes

were isolated after a 3 h induction with IPTG This

assay is effectively semiquantitative (as the cells are

again analyzed over a relatively long period) but is

more reproducible than the TorA export assay and the

pEXT22 plasmid produces TatABC at lower levels (we

estimate approximately three- to fivefold more than

wild-type [28]) Most of the data presented below

involve the use of this assay but it should be

empha-sized that all mutants were tested several times using

the both types of export assay TorA export data are

shown only where there were minor discrepancies with

the TorA-GFP data

The experimental system varied from those of

previ-ous studies [24,26] in important respects We recently

found [28] that the Tat system is inhibited by the

pres-ence of arabinose (for unknown reasons) and TorA

export assays were conducted in a slightly different

manner compared to previous studies: only 50 lm

ara-binose was used for induction (instead of 200 lm)

With the TorA-GFP export assays, TorA-GFP was induced with arabinose for 2 h, after which the arabi-nose was removed and the cells incubated with IPTG for 3 h to induce expression of the mutated tatABC operons We have found that these conditions give more reproducible results and the Tat pathway of wild-type cells is shown below to be highly active at the time of analysis

First we analyzed TatABC levels in cells expressing the various mutated subunits, and the data for the TatA and TatB mutants (expressed using the pBAD vector) are shown in Fig 1 The expression of the wild-type tatABC from the pBAD-ABC is illustrated

in the indicated lane, with wild-type cells in the adja-cent MC4100 lane; it is evident that the TatA and TatB proteins are produced from pBAD-ABC at eleva-ted levels as described above No TatC signal is evi-dent in wild-type cells because this protein is detected using antibodies to the Strep-tag II on the TatC sub-unit in the pBAD-ABC vector In the other control lane, no Tat components are detected using mem-branes from DtatABCDE cells (denoted DABCDE in Fig 1 and other figures) as expected The remaining lanes contain membrane samples from DtatABCDE cells expressing pBAD-ABC in which mutations are present in the TatA or TatB subunit as indicated

Fig 1 TatABC expression levels in cells expressing wild-type or mutated TatA ⁄ B subunits Membranes were isolated from wild-type MC4100 cells, DtatABCDE cells (DABCDE) and DtatABCDE cells expressing pBAD-ABC containing mutations in the TatA or TatB subunit as indicated Samples were immunoblotted using antibodies to TatA, TatB or the Strep-tag II on TatC Asterisks denote strains in which a Strep-tag II is not detected by immunoblotting.

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Although the expression levels vary to some extent, all

of the mutant proteins are present at similar levels,

with the possible exception of TatA⁄ G2A which

exhib-its a relatively low TatB signal for unknown reasons

One anomaly is, however, evident with two newly

gen-erated TatB mutants, E8Q and L63A: TatA and TatB

are formed at typical levels but the TatC signal is

com-pletely absent (lanes denoted by asterisks) This is

reproducible and, because these mutants display high

levels of Tat activity (see below), we assume that the

C-terminal Strep-tag II has been removed from the

proteins after expression Some of the other mutants also have this property (see below)

Although the primary aim was to analyze new mutants affected in the amphipathic or TM regions, previously analysed TatA mutants containing single amino acid changes were also analyzed in terms of their ability to export TorA and TorA-GFP, and the data for the TatA mutants are shown in Fig 2 With the TorA export assays in Fig 2A, it is observed that the bulk of the activity is found in the periplasm in wild-type cells and cells expressing pBAD-ABC, as expected (lanes P) with very little cytoplasmic signal evident TorA is found exclusively in the cytoplasm in DtatABCDE cells, where it migrates more slowly in the gel system (denoted by an asterisk) The TatA mutants all export TorA with high efficiency with the exception

of F39A, where all of the TorA is present as the cyto-plasmic form Some cytocyto-plasmic TorA is also evident with L25A

The TorA-GFP export assays are in good agreement with the TorA data (Fig 2B) In pEXT-ABC-expres-sing cells, the bulk of GFP is found as mature-size protein in the periplasm (P), whereas GFP is found only in the cytoplasm and membrane fractions (C, F)

in cells expressing the pEXT22 vector Some of this protein is present as precursor form (TorA-GFP) and some mature-size GFP is also present, presumably due to proteolytic clipping No signal is observed in DtatABCDE cells that do not synthesize TorA-GFP (a control for the specificity of the GFP antibodies) All

of the TatA mutants export TorA-GFP with high effi-ciency except F39A, which is again completely defect-ive in translocation Whereas some cytoplasmic TorA

A

B

C

Fig 2 The TatA F39A mutant is inactive whereas other TatA ⁄ B mutants show no detectable loss of translocation activity (A) Dtat-ABCDE cells expressing pBAD-ABC or the same vector containing mutations in tatA were induced using 50 lM arabinose for 3.5 h, and cytoplasmic (C) and periplasmic fractions (P) were prepared as detailed in Experimental procedures These fractions were electro-phoresed on native polyacrylamide gels that were subsequently stained for TMAO reductase (TorA) activity Asterisk denotes slower-migrating cytoplasmic form of TorA (B) A TorA-GFP con-struct was expressed in DtatABCDE cells using an arabinose-inducible vector for 2 h The arabinose was then washed out and wild-type or tatABC operons containing the same tatA mutations as

in (A) were expressed for 3 h using the isopropyl thio-b-D-galacto-side-inducible pEXT22 plasmid as detailed in Experimental proce-dures (pEXT-ABC plasmid contains wild-type tatABC operon) Cytoplasmic, membrane and periplasmic fractions (C, M, P), were isolated and immunoblotted using antibodies to GFP The mobility

of mature-size GFP is indicated (C) TatB mutants described in Fig 1 were analyzed for export of TorA-GFP (B) exactly as des-cribed in (B) for TatA mutants.

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was evident with the L25A mutation, as described

above, no defect is apparent using TorA-GFP as a

substrate Because signal strengths are not linearly

related to protein activity in the native gel TorA assay,

we are more inclined to regard the TorA-GFP data as

evidence of high translocation activity, although other

possibilities can not be excluded

Similar tests on the TatB mutants are shown in

Fig 2C The results show that all of the strains

effi-ciently export TorA-GFP, including the E8Q and

L63A mutants that exhibited no signal with the

Strep-tag II immunoblots for TatC in Fig 1

Inhibitory effects of mutations in the predicted

amphipathic regions of TatA and TatB

Considerable attention has centred on possible roles of

conserved predicted amphipathic regions that are

highly conserved in both TatA and TatB These

regions effectively bridge the transmembrane helices

and soluble cytoplasmic domains, and truncation

ana-lysis [29] has shown that they are essential for

translo-cation activity Their sequences are shown in Fig 3A

In a previous report [24], we analyzed the effects of

changing three lysine residues in TatA (residues 37, 40

and 41) to glutamine, and in a second mutant we addi-tionally changed K24 to alanine These mutants, denoted TatA⁄)3K and TatA ⁄ )4K previously [24] were shown to be active albeit with reduced efficien-cies These TatA mutants have been made (and re-named TatA⁄ 3K > Q and TatA ⁄ K24A,3K > Q) after finding several revertants in recent studies of previ-ously analyzed mutants In the case of TatB, it was previously found that changing two arginines (residues

37 and 40) to asparagine (TatB⁄ 2R > N), or three lysines (residues 65, 67 and 68) to glutamine (TatB⁄ 3K > Q) had little effect on the efficiency of Tat-dependent export [24] In the present report we have re-assessed these mutants and another mutant combining the two sets of mutations in TatB (TatB⁄ 2R > N,3K > Q) This new mutant is indica-ted by ‘’ in Fig 3 The expression profiles are shown

in Fig 3B, which shows TatA and TatB to be synthes-ized in all cases, although again at slightly varying lev-els Strep-tagged TatC is formed in every case except TatA⁄ K24A,3K > Q, but because this mutant is act-ive (see below) we again believe that the TatC protein

is present but lacking the Strep-tag II

Export assays using these mutants are shown in Fig 4A The data show that all three TatB mutants

TatA

TatA

TatB

TatC

TatA

TatB

TatC

pB AD-AB

Cs

pB AD-AB

Cs

2R>N K24AK24A K24A

3K>Q 3K>Q 2R>N 3K>Q/ 2R>N

3K>Q 3K>Q 3K>Q

3K>Q

2R>N 3K>Q 2R>N 3K>Q ∆ABCDE

∆ABCDE

TatB

16

25

30

*

A

Fig 3 Mutations in the predicted

amphi-pathic regions of TatA and TatB (A) Primary

sequences of the amphipathic regions with

the targeted residues indicated by arrows

and numbered The changes introduced in

the various mutants are indicated and

under-lined (B) pBAD-ABC cells, DtatABCDE cells

and DtatABCDE cells expressing pBAD-ABC

containing the ‘amphipathic’ mutations

shown in (A) were analyzed by

immunoblot-ting with antibodies to TatA, TatB and the

Strep-tag II on TatC Asterisks denote

strains that exhibit no signal with Strep-tag

II antibodies (C) as in (B), except with

strains expressing combinations of

tions in TatA + TatB ‘^’ denotes new

muta-tions analyzed in this study Mutamuta-tions in

TatA are shown underlined and in grey font.

Mobilities of molecular mass markers are

given on the left.

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exhibit efficient export of TorA-GFP, in that the vast

majority of protein is found in the periplasmic fraction

This includes the new TatB mutant (TatB⁄ 2R > N,

3K > Q) in which five basic residues are substituted;

surprisingly, there is little evident effect Among the

TatA mutants, TatA⁄ 3K > Q was previously described

as active [24] but Fig 4A shows this not to be the case

with the newly generated mutant, which fails to export

TorA-GFP to any detectable extent No export of TorA

was observed either (data not shown) Surprisingly, the

presence of an additional mutation (K24A) enables

export to take place, with the TatA⁄ K24A,3K > Q

quadruple mutant exhibiting moderate export activity

Some precursor form of TorA-GFP is present in the

cytoplasm and⁄ or membrane fractions but considerable

amounts of periplasmic TorA and GFP are present It is

likely that the original TatA⁄ 3K > Q mutant [24]

simi-larly acquired an additional mutation prior to analysis

that enabled translocation to occur, although this has

yet to be confirmed Other TatABC mutations described

previously [24,26] have been remade and shown to have

unchanged properties

We also expressed tatABC operons in which these multiple mutations in the amphipathic regions were combined; in the relevant Figures the TatA mutations are shown underlined for simplicity We previously reported data [24] on two such combinations: (TatA⁄ K24A, 3K > Q + TatB ⁄ 3K > Q) and (TatA ⁄ 3K > Q + TatB⁄ 2R > N), and both mutants were described as active In this report we have reassessed the effects of these mutations (as the former TatA mutant TatA⁄ 3K > Q is now known to be inactive on its own, as shown above) and have constructed several new permutations as detailed in Fig 3 These new mutations are again denoted by ‘’ Figure 3C shows that strains synthesizing all of the multiple TatAB mutations contain TatABC at similar levels and activ-ity assays are shown in Fig 4(B,C)

These ‘mixed amphipathic’ mutations exhibit very interesting properties Figures 2 and 4A showed that the TatA⁄ K24A and TatB ⁄ 2R > N mutations support wild-type levels of export activity but Fig 4B shows that the combined (TatA⁄ K24A + TatB ⁄ 2R > N) mutations severely disrupt activity, with no periplasmic

A

B

C

Fig 4 Combinations of mutations in the TatA ⁄ TatB amphipathic regions have partic-ularly severe effects on translocation activ-ity (A) Mutants containing alterations in the predicted amphipathic regions of either TatA

or TatB (as detailed in Fig 3) were analyzed for export of TorA-GFP using the assay pro-tocols detailed in Fig 2 For clarity, muta-tions in TatA are shown underlined and in grey (B) Combinations of mutations in the amphipathic regions of TatA and TatB, whose structures and expression profiles are illustrated in Fig 3, were tested for the export of TorA-GFP Mutations in TatA are shown underlined and in grey font; addition-ally, labels on the right indicate whether mutations are in TatA or TatB (C) Dtat-ABCDE cells, or DtatABCDE expressing pBAD-ABC or the same vector containing mutations in both TatA and TatB as indica-ted, were assayed for export of TorA using the protocol described in Fig 2.

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mature-size GFP detected at all after synthesis of

TorA-GFP Note that mature-size GFP accumulates in

the cytoplasm, and not the full precursor protein; this

is due to proteolytic clipping of the signal peptide

when export is blocked [28,30] Figure 4C shows TorA

export assays in which the vast majority of TorA is

found in the cytoplasm A minor fraction of TorA

is found in the periplasm, indicating that the mutant

is not completed blocked in Tat-dependent

transloca-tion, but this mutant is clearly badly compromised An

almost identical result is obtained with (TatA⁄ K24A

+ TatB⁄ 3K > Q), and it should again be noted that

the individual TatA and TatB mutants show no

appar-ent defects These data show that the mutations have

synergistic effects and the particularly severe effects on

TorA-GFP export raise the intriguing possibility that

these mutations somehow affect the export of GFP

differently when compared to TorA

The next two mutants in Fig 4B (from left to right)

contain TatA⁄ 3K > Q in combination with either

TatB⁄ 2R > N or TatB ⁄ 3K > Q Both combinations

exhibit no detectable Tat activity and this is

unsurpris-ing as we showed above that the ‘new’ TatA⁄ 3K > Q

mutant is inactive on its own Of the remaining

mutants (TatA⁄ K24A, 3K > Q + TatB ⁄ 3K > Q) is

completely inactive, although the individual TatA and

TatB mutants did exhibit activity, and the final mutant

containing five changes in TatA plus four in TatB is

likewise totally inactive In all, these mutants

empha-size the importance of the amphipathic region but they

also show for the first time that combinations of

TatA⁄ TatB mutations can have far more dramatic

effects than the individual mutations

Mutations in the transmembrane spans

of TatA and TatB

Deletion of the TM spans of TatA or TatB leads to a

loss of activity [31] but the important characteristics of

these regions have not been probed We constructed

a series of new TatA⁄ B mutants containing changes

within the TM spans, for two reasons First, it has

been suggested that TatA may form the translocation

channel, in which case drastic structural alterations

may be expected to selectively block the translocation

event Secondly, mutations affecting the structure and

orientation of the TM span may be expected to disrupt

the interactions with other Tat components, and this

would provide information on the inter-subunit

associ-ations occurring within and between Tat complexes

Both of these areas are poorly understood at present

It has been shown with other proteins that the

intro-duction of proline residues has a marked effect on the

structures of TM spans [32,33], usually introducing dis-tortions of major proportions, and such substitutions were made in the TM spans of TatA and TatB in the present study We also substituted three residues in the TatA and TatB TM spans by glycine The presence

of glycine can also lead to increased flexibility in TM helices [34] However, glycine residues can also play important roles in modulating inter-helix interactions [35] and the effects of inserting or removing these resi-dues may therefore be less predictable than with pro-line mutations Nevertheless, the presence of three consecutive glycines should lead to a significant struc-tural effect in either case The proline and glycine sub-stitutions were made near the centre of the TM span

in order to maximize possible structural effects Figure 5A shows the sequences of the TatA and TatB TM spans, together those of the mutated forms With TatA, residues 11–13 were changed to glycine in one case (TatA⁄ 3Gly) and a single residue was chan-ged to proline in the centre of the TM span in another (TatA⁄ I12P) We also changed three additional residues to proline in the TatA⁄ 3Gly mutant (TatA ⁄ 3Pro3Gly) and then a further three residues to glycine

in the same subunit (TatA⁄ 3Pro6Gly) With TatB, resi-dues 11–13 were changed to glycine (TatB⁄ 3Gly) or a single residue to proline (TatB⁄ V12P)

The expression characteristics of these mutants are shown in Fig 5B With the simplest TatA mutants, TatA⁄ 3Gly and TatA ⁄ I12P, TatABC are all present

at expected levels With TatA⁄ 3Pro3Gly, TatA and TatB are present at the usual levels but TatC is not detected at all However, as this mutant is highly act-ive (see below) it appears that this is another example

of the C-terminal Strep-tag II being clipped or modi-fied With the most drastic of the TatA mutants, TatA⁄ 3Pro6Gly, TatB and TatC are synthesized but

no TatA is detected Fractionation of cells synthes-izing TatA⁄ 3Pro3Gly shows the presence of full-length protein in the cytosol, consistent with a slight defect in membrane-insertion; in contrast, smaller fragments of the TatA⁄ 3Gly6Pro protein are found in the cytosol (data not shown) This suggests that the TatA⁄ 3Gly6Pro protein is degraded either within the membrane or, perhaps more likely, after failure to insert into the membrane

Cells expressing the simpler of the tatB mutants, TatB⁄ V12P, appear to contain TatABC at expected levels but the TatB⁄ 3Gly mutations result in a much-reduced TatB signal, presumably reflecting problems in insertion and⁄ or stability No TatC signal is evident, but this again appears to reflect problems in detection

of the Strep-tag II as this mutant is active in Tat-dependent transport (see below)

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Figure 6 shows TorA and TorA-GFP export assays

for these TM span mutants Of the TatA mutants,

TatA⁄ I12P shows no detectable defect because GFP

and TorA are found predominantly in the periplasm

The TatA⁄ 3Gly mutant, on the other hand is blocked

in export and no translocation activity can be detected

The same applies to the TatA⁄ 3Pro6Gly mutant,

although this is expected because the immunoblots in

Fig 5 show no signal for TatA The real surprise is

the TatA⁄ 3Pro3Gly mutant, which is shown to export

both TorA and TorA-GFP with high efficiency Given

that the parent TatA⁄ 3Gly mutant is completely inac-tive, this result indicates that the three proline residues somehow compensate for the inhibitory effects of the glycine residues and enable translocation to occur Finally, Fig 6 shows that the two TatB mutants, TatB⁄ 3Gly and TatB ⁄ V12P, are highly active in export; perhaps surprisingly given the drastic effects of the 3Gly mutations in TatA

We also tested the effects of expressing tatABC operons carrying combinations of these mutations in the TM spans of both TatA and TatB, namely (TatA⁄ 3Gly + TatB⁄ 3Gly) (TatA ⁄ 3Gly + TatB ⁄ V12P) (TatA ⁄ I12P + TatB⁄ 3Gly) and (TatA ⁄ I12P + TatB ⁄ V12P) Immunoblots confirmed that the TatABC were syn-thesized at approximately the same levels as the wild-type subunits generated from pBAD-ABC (data not shown), and activity assays are shown in Fig 7 With the TorA assays, the control tests show efficient export with wild-type TatABC and a complete block in export

in the tat null mutant (denotedDABCDE), as expected The combination of (TatA⁄ 3Gly + TatB ⁄ 3Gly) is blocked in Tat function, and this is not unexpected given that the TatA⁄ 3Gly mutant itself shows no export activity However, a combination of (TatA⁄ 3Gly + TatB⁄ V12P) displays very efficient export of TorA and this shows that the TatB⁄ V12P mutation compensates for the drastic effects of the 3Gly muta-tions in TatA This is confirmed by the TorA-GFP export assays, which reveal a complete block in export with the (TatA⁄ 3Gly + TatB ⁄ 3Gly) mutant but near wild-type export efficiency with (TatA⁄ 3Gly + TatB ⁄ V12P) The remaining (TatA⁄ I12P + TatB ⁄ 3Gly) and (TatA⁄ I12P + TatB ⁄ V12P) mutants export both TorA and TorA-GFP efficiently, in keeping with the finding that none of the mutations affect export to a detect-able extent when present in TatA or TatB alone (see Fig 6) In conjunction with the data shown in Fig 6, these data show that the severe effects of the TatA⁄ 3Gly mutations can be rescued by the presence

of additional mutations either elsewhere in the TatA

TM span or in the TatB TM span (TatB⁄ V12P mutation)

Mutagenesis of TatC TatC has also been studied in previous reports and a number of mutations have been characterized [26,27], but some apparent differences were reported in studies

on the same mutants by different groups (see below) Few TatC residues are highly conserved but of these, a high proportion is clustered in the N-terminal cyto-plasmic domain and the first cytocyto-plasmic loop In our previous analysis [26] only two residues were found to

A

B

Fig 5 Expression of TatA and TatB mutants containing alterations

in the transmembrane spans (A) Sequences of the TM regions of

TatA and TatB, with residues numbered and the substitutions

indi-cated (B) Expression of the various mutations constructed within

the pBAD-ABC vector Samples were analyzed by immunoblotting

with antibodies to TatA, TatB and the Strep-tag II on TatC

Mobili-ties of molecular mass markers are given on the left.

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be absolutely essential for TatC function: R17A (N-terminal cytoplasmic region) and P48A (first peri-plasmic loop) The deletion of three residues (20–22) also disrupted function, prompting the suggestion that this cytoplasmic domain played an important role In

a separate study [27], R17 was again found to be important but two acidic residues, E103 and D211 were found to be particularly critical; E103A⁄ Q ⁄ R mutants and D211A were completely inactive, although D211E⁄ N mutants were partially active These residues are located on the first cytoplasmic loop and third periplasmic loop, respectively Substitution

of F94 (at the interface between cytoplasmic loop I and the membrane bilayer) was also reported to block transport activity [27] D211 was not analyzed in our previous study [26] but we did find that E103A showed

no translocation defect at all, and so we have made new mutants in all three residues in order to analyse the effects using our expression and assay systems

As with other mutants, we carried out expression studies using all of the TatC mutants; in each case the TatABC subunits were present at similar levels and in

A

B

Fig 6 Effects of mutations in the TM

regions of TatA and TatB The TatA and

TatB mutants containing alterations in TM

spans (detailed in Fig 5) were tested for

effects on translocation activity (A)

Muta-tions within the pBAD-ABC vector were

assayed for export of TorA (B) mutations

within pEXT-ABC were assayed for export

of TorA-GFP, as detailed in Fig 2 Cells

expressing pBAD-ABC or pEXT-ABC without

mutations were analyzed as controls, and

DtatABCDE cells were analyzed for export

of TorA, again as a control Other symbols

are as in Fig 2.

A

B

Fig 7 A mutation in the TatB TM span can compensate for the

severe effects of the TatA ⁄ 3Gly mutation This figure illustrates the

translocation activities of four DtatABCDE strains expressing

pBAD-ABC or pEXT-pBAD-ABC in which mutations are present in the TM spans

of both TatA and TatB (mutations in TatA are shown underlined and

labels on the right indicate whether the mutations are in TatA or

TatB) Cells were analyzed for the export of TorA (A) or TorA-GFP

(B) using protocols described in Fig 2.

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these instances the TatC Strep-tag II were all found to

be intact (data not shown)

Mutations in the first cytoplasmic loop are

charac-terized in Fig 8(A) None of these mutants display

any detectable defects in translocation efficiency,

inclu-ding the E103A and E103Q mutants which do not

even contain elevated levels of the precursor protein

TorA-GFP These data do not agree with reports that

the two residues are critical [27], and with this

appar-ent contradiction in mind we made each mutant again

and again found them to be highly active (data not

shown) Figure 8(B) shows the effects of mutations in

TM spans two to six Most of these mutations again

have no detectable effect with the notable exception of

F94A which is completely inactive These results agree

with those reported in [27]

The final study on TatC is shown in Fig 9, where

mutations in the periplasmic loops are analyzed We

have previously shown that the P48A mutation

des-troys activity, and the data confirm this result with no

export detected using either assay system The K73A

and Y154S mutants are active, as expected from

previ-ous studies [26] and so too are the D211A and D211N

mutants that were described as completely or partially

inactive, respectively, in a previous study [27] In Fig 9, no translocation defects are apparent with either D211A or D211N and these mutants were again

A

B

Fig 8 Mutations in several residues of the cytoplasmic loops in TatC cause no detect-able loss of translocation activity (A) TatC mutants carrying substitutions in the 1st cytoplasmic loops were tested for export of TorA-GFP as described in Fig 2; mutations were made within the pEXT-ABC vector and the Figure shows assays using pEXT-ABC

as a control (B) Similar tests carried out using TatC mutants carrying substitutions in

TM spans (numbered above the lanes).

A

B

Fig 9 Effects of mutations in the periplasmic loops of TatC Muta-tions in the three periplasmic loops of TatC (numbers indicated above the lanes) were assessed using export assays for TorA (upper panel) or TorA-GFP (lower panel) as described earlier for other mutants (Fig 2).

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