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Mechanical interactions at the levels of cells, organs and organisms are responsible for such familiar physiological functions as motor function, hearing [18], touch [19], and the regula

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sensor for specific proteins in situ

Fanjie Meng, Thomas M Suchyna and Frederick Sachs

Center for Single Molecule Biophysics, Department of Physiology and Biophysics, State University of New York at Buffalo, NY, USA

Mechanical stress is one of the most influential

physical factors in biology and one of the least

charac-terized Whereas it is obvious from molecular

dyna-mics [1–4] and force spectroscopy [5–12] that forces

deform molecules, the mechanics of cells are much

more complicated, involving the interaction of

hetero-geneous polymers and membranes and their interaction

with both two-dimensional heterogeneous liquid

mem-branes [13,14] and three-dimensional cytoplasmic

solu-tions, where signaling factors can vary in time and

space [15–17] Mechanical interactions at the levels of

cells, organs and organisms are responsible for such familiar physiological functions as motor function, hearing [18], touch [19], and the regulation of blood pressure [20], but the interactions are also deeply embedded in the biochemistry of the cell, affecting such varied processes as the phenotype of stem cells [21], DNA transcription [22,23], translation of cellular components by motor proteins such as kinesin [5], stress-induced changes of structure, such as occur in shear stress modulation of the cytoskeleton of the endothelia [24,25], and more general interactions due

Keywords

Cerulean; fluorescence resonance energy

transfer; relative orientation factor; Venus;

a-helix linker

Correspondence

F Sachs, Center for Single Molecule

Biophysics, Department of Physiology and

Biophysics, State University of New York at

Buffalo, 3435 Main Street, Buffalo, NY,

14214 USA

Fax: +1 716 829 2569

Tel: +1 716 829 3289 ext 105

E-mail: sachs@buffalo.edu

(Received 15 December 2007, revised 9

April 2008, accepted 11 April 2008)

doi:10.1111/j.1742-4658.2008.06461.x

To measure mechanical stress in real time, we designed a fluorescence reso-nance energy transfer (FRET) cassette, denoted stFRET, which could be inserted into structural protein hosts The probe was composed of a green fluorescence protein pair, Cerulean and Venus, linked with a stable a-helix

We measured the FRET efficiency of the free cassette protein as a function

of the length of the linker, the angles of the fluorophores, temperature and urea denaturation, and protease treatment The linking helix was stable to

80C, unfolded in 8 m urea, and rapidly digested by proteases, but in all cases the fluorophores were unaffected We modified the a-helix linker by adding and subtracting residues to vary the angles and distance between the donor and acceptor, and assuming that the cassette was a rigid body,

we calculated its geometry We tested the strain sensitivity of stFRET by linking both ends to a rubber sheet subjected to equibiaxial stretch FRET decreased proportionally to the substrate strain The naked cassette expressed well in human embryonic kidney-293 cells and, surprisingly, was concentrated in the nucleus However, when the cassette was located into host proteins such a-actinin, nonerythrocyte spectrin and filamin A, the labeled hosts expressed well and distributed normally in cell lines such as 3T3, where they were stressed at the leading edge of migrating cells and relaxed at the trailing edge When collagen-19 was labeled near its middle with stFRET, it expressed well in Caenorhabditis elegans, distributing simi-larly to hosts labeled with a terminal green fluorescent protein, and the worms behaved normally

Abbreviations

CFP, cyan fluorescent protein; COL-19, collagen-19; D ⁄ A ratio, donor emission to acceptor emission ratio; DIC, differential interference contrast; E, fluorescence resonance energy transfer energy transfer efficiency; FRET, fluorescence resonance energy transfer; GFP, green fluorescent protein; HEK, human embryonic kidney; YPF, yellow fluorescent protein.

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to the physical chemistry of concentrated protein

solu-tions [26] To dissect which stresses affect which

func-tions, we need labels that are sensitive to mechanical

stress and that can be attached to specific proteins

To meet that need, we designed a cassette

(denoted stFRET) that can be inserted into

struc-tural proteins and reports molecular strain via

changes in fluorescence resonance energy transfer

(FRET), and, with appropriate calibration, molecular

stress The cassette consists of the green fluorescent

protein (GFP) monomers Cerulean and Venus

[27–31], linked by a stable a-helix [32] This article

characterizes the properties of the probes, and shows

that they can be efficiently incorporated into

struc-tural proteins such as collagen-19 (COL-19),

nonery-throcyte spectrin, a-actinin and filamin A within

living cells, and that the FRET from this cassette

changes with stress in situ

The efficiency of energy transfer for a FRET pair

is E 1 ⁄ [1 + (R ⁄ RO)6], where R is the distance

between the dipoles and RO is the characteristic

distance for 50% energy transfer [33] The maximal

sensitivity for changes in R occurs at R = RO For

Venus and Cerulean, RO is  5 nm [34], so we linked

them with a 5 nm a-helix The efficiency is affected

by the angle between the transition dipoles as well as

the distance between them, and we estimated the

probe geometry by varying the number of residues in

the linker Removing one residue caused a large

change in angle with a small change in distance, and

adding or removing a full turn produced a change in

distance with no change in angle We used six

mutants to solve for the three relevant angles of the

dipoles, assuming that the cassette was rigid stFRET

was stable over temperature and mild urea denaturing

conditions, but with 8 m urea, the linker unfolded

and the fluorophores remained stable Thus, stFRET

is robust

stFRET expressed well in various biological systems,

including 3T3 and human embryonic kidney

(HEK)-293 cells and in Caenorhabditis elegans After insertion

into a variety of structural host proteins such as

colla-gen, filamin, actinin and spectrin, it distributed in the

same manner as the same hosts with terminal GFP

tags stFRET changed FRET with the spontaneous

movement of motile cells, decreasing efficiency in

regions under tension and increasing it in regions

expected to be free of significant stress By axially

stretching C elegans, we could demonstrate acute

reversible changes in FRET associated with tension

and relaxation stFRET opens the door to studying in

real time many physiological processes that are

modu-lated or driven by mechanical stress

Results

General configuration and FRET spectra of stFRET and its variants

Figure 1 is a diagram of stFRET geometry as deduced from the procedure described in Modeling and calibra-tion in the Experimental procedures Figure 2A shows the general configuration of six stFRET variants The inward arrows show the excitation wavelength, and the outward arrows show the emission wavelength Width

of arrows denotes light intensity Figure 2B shows the alignment of the DNA sequence of the linker with five modified versions (the predicted geometrical changes are shown in Table 1) As shown in Table 1, according

to the general property of a-helices, one amino acid deletion produces a change ()100) in angle with negli-gible change ()1.5 A˚) in length A five residue deletion

of the helix rotates the structure by 360 but shrinks the helix by 2.7 nm Deletion or addition of two and a half turns of the helix twists the structure by)180 or +180 and decreases or increases the length by 1.35 nm Figure 2C gives the amino acid sequence and the segments of the helix linker that we modified Deletion of 18 amino acids eliminates five turns of the helix, and a nine amino acid deletion eliminates two and half turns

Figure 3A shows the emission spectrum of stFRET with excitation at 433 nm There are peaks at 475 nm

Table 1 Changes in stFRET geometry caused by adding and delet-ing amino acids Positive symbols indicate an increasdelet-ing amount, and negative symbol indicate a decreasing amount.

No amino acids added or subtracted

Change in length

of linker (nm)

Change in angle

of linker (radians)

Fig 1 Geometry of stFRET D and A are donor and acceptor dipole vectors, and r is the length of the linker The three angles (h A , h D , U) are the unknown parameters R A–D is the distance between acceptor and donor chromophores.

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and 527 nm, with the 475 nm emission from the donor

Cerulean and 527 nm from the acceptor Venus having

robust energy transfer A 100 lm solution of unlinked

donor and acceptor (1 : 1 mixture, green filled squares

and line with 433 nm excitation) had a small emission

at 527 nm due to the bleed-through from Cerulean,

the donor (blue filled inverted triangle and line) and

some direct excitation of the acceptor Venus by

433 nm (black triangle and line) The donor and

accep-tor mixture had E = 0 and donor emission to accepaccep-tor

emission ratio (D⁄ A ratio) = 2.47 ± 0.05 (Fig 3B)

However, for stFRET, E = 44 ± 2.5% and D⁄ A

ratio = 0.47 ± 0.02, showing efficient energy transfer (for E and D⁄ A ratio calculation, see Experimental procedures)

Calibration of three angles and j2

Confident in the origin of stFRET energy transfer, we purified the other five variants and measured their flu-orescence (Fig 4A) All mutants exhibited robust FRET (Table 2) stFRET itself had 44 ± 2.5% energy transfer, and the 5T construct had the highest effi-ciency, E = 56 ± 4.5%, the 2.5T construct increased

A

B

C

Fig 2 Construction of stFRET protein and five variants (A) Schematic structure of stFRET Cyan is the donor, Cerulean; yellow

is the acceptor, Venus The height of the b-can structure is 4.2 nm The black helix is the linker, and it nominal length is 5.0 nm Incoming arrows indicate excitation, and outgoing arrows indicate emission, with the wavelength marked next to them; the width

of the arrows is proportional to the light intensity (B) Alignment of the primary and modified linker DNA sequences (C) Modifi-cations to the linker with DNA and amino acid sequences.

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E to 47 ± 2.1%, whereas the 2.5I construct decreased

E to 37 ± 0.9% FT1AA and FT2AA, presumably

only having their angles changed, decreased E to

29 ± 7.1% and 38 ± 4.3%, respectively (Fig 4B)

Table 2 summarizes the apparent change of angles and

distances obtained by modifying the linker and the

corresponding energy transfer efficiency

If we assume that a single residue alters the linker

length by a translation of 0.15 nm and 100, and that

the structure is rigid, we can use the data in Table 2 to

solve for the probe geometry (see Experimental

proce-dures) The numerical solutions gave hA= 3.83,

hD=)0.78 and U = 1.97 radians, and j2= 0.86,

which is 30% higher than 2⁄ 3, the j2value that one

would obtain assuming random rotation of the donor

and acceptor (Fig 1) However, it should be pointed

out that a value of j2 2 ⁄ 3 does not necessarily imply

that the probes are moving randomly

Stability of the linker as perturbed by urea,

temperature, and proteinase K

We did a number of tests to assess linker integrity If

the linker was an a-helix, then melting would increase

the end–end spacing and the efficiency would decrease

With urea as a denaturant [35,36], Fig 5A shows that

the efficiency of stFRET declined with concentration

up to 8 m, and the previously quenched donor

emis-sion recovered Remarkably, the fluorophore spectra

were almost unaffected by urea, with < 10–15%

change in amplitude (Fig 5C,D) Figure 5B shows

that 1–8 m urea caused the D⁄ A ratio to increase

from 0.46 to 1.21, as expected if the helix unfolded

into a random coil allowing the donor and acceptor to

move further apart and reducing energy transfer

(Fig 5E)

As a second test of the helix stability, we tried to

melt stFRET at elevated temperatures, but the protein

proved stable up to 80C Figure 6A shows the

tem-perature dependence of fluorescence of 100 lm

stFRET protein excited at 433 nm from room

temper-ature to 80C Donor and acceptor emission both

declined somewhat as the temperature increased,

prob-ably due to a direct change in quantum efficiency, but

there was no significant change in transfer efficiency

from 60C to 80 C, the upper limit of our

measure-ments, so that the linker structure can be considered to

be quite robust

As a final test of linker integrity, we digested

stFRET with proteases that cut the linker but left the

fluorophores intact Figure 7 shows that proteinase K

led to a rapid fall in efficiency that was complete

within 1 min The D⁄ A ratio changed from 0.42 to

1.95 over 30 min (Fig 7B), as compared to a change from 0.46 to only 1.21 when the protein was treated with 8 m urea (Fig 5B) Similar behavior was found for all six constructs (data not shown) The donor and acceptor fluorophore spectra were unaffected by pro-teinase K after 30 min of digestion (Fig 7C,D) Figures 5E and 7E are diagrammatic models summa-rizing the energy transfer between donor and acceptor under different treatments (the width of the arrows represents signal intensity)

In vitro measurement of strain sensitivity

To verify the strain responsiveness, we bonded the ends of derivatized stFRET to a silicone rubber sheet using StreptagII–Streptactin and stretched the sheet equibiaxially on the fluorescence microscope When the C-terminal and N-terminal ends of stFRET were derivatized so that it would be stretched with the sheet, there was a reversible  11% decrease in the D ⁄ A ratio (Fig 8) As a control, we measured FRET from stFRET that was derivatized at one end only so that it was simply immobilized but not stretched and there was no significant change in FRET with strain (Fig 8) Nonspecific binding of double-tagged stFRET

to an untreated silicone surface also produced no sig-nificant change in FRET with strain Thus, stFRET is sensitive to strain, as expected from the solution assays and the design of the probe

Eukaryotic expression and targeting property

of stFRET Before inserting stFRET into host proteins, we placed the gene under a eukaryotic promoter (human cyto-megalovirus) and transiently transfected HEK cells with stFRET alone Control transfections with Venus

or Cerulean monomers showed no preferential locali-zation and no obvious energy transfer (Fig 9A–F) Cells transfected with stFRET displayed significant energy transfer (Fig 9I) stFRET localized to the nucleus with an extremely high density in the nucleoli (Fig 9K)

Nuclear targeting proteins have a consensus amino acid sequence of lysine⁄ arginine [K ⁄ R(4–6)] or smaller clusters separated by 10–12 amino acids: [K⁄ R(2)X(10–12)K ⁄ R(3)] [37] The linker has multiple arginine clusters similar to the nuclear targeting sequence, but simply removing one or the other fluoro-phores from stFRET produced a uniform cytoplasmic distribution showing that the linker’s sequence alone was not sufficient for targeting These unexpected nuclear targeting properties of stFRET may provide

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a useful tool for understanding nuclear protein

transport

Host proteins of stFRET with normal expression

showing stress sensitivity

We inserted stFRET into various host proteins,

inclu-ding COL-19 (Fig 10G), nonerythrocyte spectrin

(Fig 10E), filamin A (Fig 10C), and a-actinin

(Fig 10A), and expression systems including HEK-293,

3T3 and C elegans, and the insertion locations were

optimized to obtain protein distributions similar to

those observed for the host protein C-terminus tagged

with GFP or Cerulean (Fig 10B,D,F,H) Inserting

stFRET into host proteins eliminated nuclear targeting

The fluorescence of stFRET in cultured cells was

located in the cytoplasm and⁄ or the cell membrane, depending on the host (Fig 10A,C,E) We expressed the construct of the most abundant collagen in C elegans, COL-19, and the protein was properly assem-bled, showing the typical striated pattern, and the worms behaved normally When we stretched the worm with micromanipulators, the labeled COL-19 showed a decrease in FRET efficiency with stretch, and in convex regions as it actively wiggled (Fig 10G,H)

Figure 11 indicates that stFRET integrated into actinin and filamin can sense tension in situ Migrating

A

B

C

Fig 4 Modification of the linker change FRET efficiency of six con-structs (A) Fluorescence spectra of stFRET and its five variants (scan parameters as in Fig 3) (B) FRET efficiency of the six con-structs (C) SDS ⁄ PAGE gel of the purified proteins, and Cerulean and Venus monomers FT stands for stFRET; 5T and 2.5T are con-structs with five-turn or 2.5-turn deletions from the linker; 2.5I is the construct with a 2.5-turn insert; FT1AA and FT2AA are the con-structs with one amino acid or two amino acid deletions All values are means ± SD, and the data were obtained with proteins from three separate purifications.

A

B

Fig 3 FRET efficiency and D ⁄ A ratio (mean ± SD) (A) Spectra of

stFRET, Cerulean and Venus monomers and Cerulean and Venus in

a 1 : 1 mixture Venus + Cerulean mixture, green filled squares.

Donor Cerulean, blue inverted triangles and line Acceptor Venus,

black triangles and line Pure stFRET protein, red filled circles and

line (B) FRET efficiency and D ⁄ A ratio of stFRET with Cerulean

and Venus in a 1 : 1 mixture Data were obtained with protein from

three separate purifications CV is Cerulean and Venus in a 1 : 1

mixture FT, stFRET Excitation 433 nm; emission 460–550 nm.

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3T3 cells have a characteristic leading and lagging

edge, and Fig 11A–C shows the donor, acceptor and

FRET images from three confocal microscopy

chan-nels stFRET was distributed evenly across the cyto-plasm as visualized with a 16-color pseudocolor map (Fig 11C,D) Transfection with actinin–stFRET

Table 2 Values of parameters in Eqn (8) of six stFRET variants as described in Fig 4.

Protein

constructs

Energy transfer

efficiency (E) (%)

r (linker length) (nm)

Z (H ⁄ 2 of b-Can) (nm)

h A (unknown parameter 1)

h D (unknown parameter 2)

U (unknown parameter 3)

Fig 5 Melting the linker (A) Spectra from

stFRET treated with 1–8 M urea (scan

parameters as in Fig 3B) (B) D⁄ A ratio of

stFRET after treatment with different

con-centrations of urea (means ± SD, n = 3 in

each treatment); increasing D ⁄ A ratio

indi-cates the recovery of donor emission and

decrease of energy transfer (C) Cerulean

monomer fluorescence with urea

treat-ments (scan parameters as in Fig 3) (D)

Venus monomer fluorescence with urea

(excitation at 515 nm and scan 520–

600 nm) (E) Urea melts the linker and

leaves the donor and acceptor intact,

decreasing FRET energy transfer as donor

emission recoverers and D ⁄ A ratio increases

(definitions as in Fig 2A).

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revealed that during migration, the lagging edge

showed higher energy transfer than the leading edge

(Fig 11E,F), i.e it was relaxed We measured the

effi-ciency of various domains in the lagging and leading

edges from 14 confocal image stacks The lagging

edges (the red-outlined domain) nearly doubled the

FRET efficiency as compared to the leading edge

(blue- and green-outlined domains) Multiple cells had

the same behavior, but because of the complexity of

the various shapes it was difficult to arrive at any

use-ful statistic for frequency We have shown a typical

cell with different domains as an internal control The

same phenomenon was observed in

filamin–stFRET-transfected 3T3 cells (Fig 11G–L) Figure 11G–I

shows three confocal image channels, and Fig 11J is

the pseudocolor image of stFRET protein distribution

Figure 11K is the FRET efficiency image in which three domains were selected The efficiency in the red-outlined domain is twice as high as that in the blue and green domains (Fig 11L) These data suggest that tension in both actinin and filamin is lower in domains close to the lagging edge (where adhesion to the sub-strate is released), and higher at the leading edge where adhesions pull the cell forward

Discussion

Designed to be an in situ stress sensor, stFRET has robust and predictable energy transfer both in vitro and in vivo We were able to explore the geometry of stFRET by perturbing the linker length and terminal angles using the known properties of a-helices FRET efficiency changed in a predictable manner with the postulated geometry, suggesting that the fluorophores are not free to rotate A recent molecular dynamics simulation study of FRET in lysozyme found that j and ROcould be correlated by as much as 0.8, so that FRET measurements that assume random rotational freedom are likely to be in error [38] The ability to change angle and distance by varying the linker can be used in vivo to examine the effect of host proteins on probe geometry Regardless of the coupling of the flu-orophores to the linker, all of the host proteins that

we studied were coiled-coiled dimers or trimers, so that the fluorophores of stFRET would not be able to rotate freely

Figure 2A shows the predicted mean structure of free stFRET The three unknown angles of Eqn (8) (see Experimental procedures) were solved using data for the six mutants using the least squares equation solver in maple The solutions were stable to perturba-tions of the starting values, suggesting that we were measuring a constrained system Our final solution was

hA= 3.83, hD=)0.78, and U = 1.97, yielding

j2= 0.86 There will be bending and flexing motions

of the structure in solution, but we obtained consistent answers from the overdetermined set of equations, sug-gesting that the calculated mean values are at least self-consistent The geometric values that we have cal-culated would represent mean values weighted by the efficiency Fluctuations that bring the dipoles closer are more heavily weighted than those that move them further away, although the probability of occupancy of these conformations is another weighting factor A detailed molecular dynamics simulation would be use-ful, but is not essential for the use of stFRET as a probe of molecular stress, as the most important vari-ables are the differences in efficiency, i.e the gradients

of stress

A

B

Fig 6 a-Helix linker in stFRET is resistant to temperature melting.

(A) stFRET spectra obtained at 60 C for 2 min, 60 C for 5 min,

70 C for 5 min and 80 C for 5 min (scan parameters as in Fig 3).

(B) stFRET D ⁄ A ratio after different temperature treatments

(means ± SD, n = 3 in each treatment) Temperatures are given in

degrees Celsius; roomtem, room temperature.

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The robust nature of stFRET was clear from the

melting experiments stFRET was thermally stable up

to at least 80C, with the FRET efficiency being

virtu-ally unchanged Melting the linker with urea (Fig 5)

[39] left the fluorophores untouched (Fig 5C,D), but

decreased the energy transfer, consistent with

unfold-ing of the linker (Fig 5B,E) Two models have been

proposed for urea-induced protein denaturation: the

binding model, in which the denaturant binds weakly

but specifically to sites exposed by the unfolded

pro-teins [40], and a solvent exchange model, in which the

interaction of the solvent and the denaturant is a

one-for-one substitution reaction at particular sites [41]

stFRET might serve as a useful probe to examine these

alternatives

The sensitivity of stFRET to protease cleavage has

both positive and negative implications If proteases

are accidentally present in situ, they could cleave

stFRET and provide misleading results We saw no evidence of protease activity in HEK or 3T3 cells

or C elegans However, the presence of intracellular proteases has been associated with acute pancreatitis, proposed to arise from trypsin overactivation in large endocytotic vacuoles of acinar cells [42] Thus, to study pancreatitis, stFRET may be a useful probe (Fig 7)

Having established the basic physical properties of stFRET, we expressed it in HEK cells (Fig 9) and evaluated the energy transfer by Xia’s method [43], using confocal microscopy The surprising localization

of stFRET to the nucleus was proved not to be a result of the linker possessing a consensus nuclear tar-geting sequence, as deletion of either fluorophore from the construct destroyed localization This adaptability suggests that stFRET can serve as a useful probe of nuclear targeting

Proteinase K

C

E

D

Fig 7 Two units of proteinase K

(1 unitÆlL)1) digests the linker but not

Cerulean or Venus (A, C, D) Spectra of

stFRET protein (A), Cerulean (C) and Venus

(D) digested for 20 s, 1 min, 2 min, 3 min,

5 min, 10 min, 15 min and 30 min at room

temperature with 200 lL of 100 l M protein.

(B) Time course of D ⁄ A ratio for

protein-ase K digestion of stFRET (E) Proteinprotein-ase K

cleaved the linker and eliminated FRET

in stFRET protein PK, proteinase K; S,

seconds; M, minutes; n = 3.

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Knowing how native stFRET itself distributes,

we incorporated it into host proteins, including nonerythrocyte spectrin, filamin A and a-actinin (Fig 10A,C,E) in 3T3 cells, and COL-19 in C elegans (Fig 10G) The distribution of the probe depended upon where the cassette was placed within the host When it was inserted towards the middle, the fluores-cence distribution appeared similar to that of the host protein tagged with GFP or cyan fluorescent protein (CFP) at the C-terminus (Fig 10B,D,F,H) Insertion

of the cassette towards the termini of the host led to different spatial distributions There is no gold stan-dard for the proper localization of proteins in cells, as fixation and exposure to various tracer ligands can produce changes in structure, but, to first order, the stFRET probes placed in the middle of the hosts appeared to cause minimal perturbation

Under physiological conditions, FRET efficiency varied in different regions of the cells (Fig 11), and these seemed to be correlated with the anticipated distribution of stress Efficiency should be reduced when the host is under tension Actinin–stFRET and filamin–stFRET generally showed lower efficiency than free stFRET (Fig 3B), suggesting that those proteins were normally under tension (Fig 11E,F,K,L,

green-1.5

2.0

2.5

3.0

Untreated - double Strep-Tag2 Strep-tactin treated - double Strep-Tag2 Strep-tactin treated - single Strep-Tag2

11%

1 s

100 mmHg

Fig 8 Double Streptag II-tagged stFRET shows a decrease in

FRET ratio when stretched on silicone rubber disks Single and

dou-ble Streptag II-tagged stFRETs were allowed to bind to either

untreated or Strep-tactin-modified silicone disks The FRET ratio

was monitored in 10 spots on each disk during application of the

suction stimulus shown Only the disks with Strep-tactin-treated

surfaces and stFRET proteins with Streptag tags at both the

C-ter-minus and N-terC-ter-minus showed a significant change in FRET ratio

when stretched.

Fig 9 stFRET expressed in HEK-293 cells exhibits efficient FRET (A–C) Confocal refer-ence image of Cerulean taken from the CFP channel (A) and the DIC channel (B), with the overlap in (C) (D–F) Reference image of Venus from the YFP (D) and DIC channels (E), with the overlap in (F) (G–K) Images of stFRET using the CFP channel (G), YFP channel (H), FRET channel (I) and DIC nel (J), with the overlap of these four chan-nels in (K) (L) The vFRET index was calibrated pixel by pixel using Xia’s method [43] Hollow black regions were excluded from the calculation because of intensity saturation stFRET is localized in the nucleus and especially concentrated in the nucleoli (arrowheads).

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line and blue-line domains) However, as cells migrate,

the stress in the leading and trailing edges changes

Connections to the extracellular matrix in the lagging

edge must be disengaged and the connections at the

leading edge put under tension Figure 11E,F,K,L

shows increased FRET efficiency in the lagging edge

as the filopodia were released from the substrate and

tension decreased (red-line domains), and decreased

efficiency associated with increased tension in the lead-ing edge as the cell was pulled forward

To turn stFRET from a strain sensor into a stress sensor, we need to measure its force–distance properties

At the current time, we only have estimates from pub-lished atomic force microscopy data on the stretching

of the coiled-coil myosin II [44] Schweiger et al [45] obtained a three-phase force–distance relationship: a linear phase of 1 mNÆm)1, a plateau of 25 pN, and

a wormlike chain phase as the helices were stretched closer to the contour length The presence of a force plateau implies that if monomeric stFRET was sub-jected to a force of > 10–25 pN, it would unfold in an all-or-none manner for about 3 nm, producing a large drop in FRET We do not see this, probably in part because the in situ probes are not homomers, but are coiled coils where the stress is shared with labeled and unlabeled neighbors It may be possible to knock down the background hosts to at least create homogeneously labeled hosts In addition, stress is shared between different proteins within the cell, and at the current time, we are only probing one of those components stFRET can be applied to any biological system with large covalently bonded proteins It is possible to examine the role of stress in selected proteins within cells or even within free-ranging organisms With organ targeting in small organisms such as C elegans and zebrafish, it should be possible to develop high-contrast video images of specific parts of the organism during controlled or natural behavior We look for-ward to finding out how mechanical stress is coupled

to biochemistry and to cell biology

Experimental procedures

Gene construction and protein purification pEYFP-C1 Venus and pECFP-C1 Cerulean plasmids were generous gifts from D W Piston (Department of Molecular Physiology and Biophysics, Vanderbilt University Medical Center, Nashville, TN, USA) [45] The Cerulean gene was subcloned from pECFP-C1 with the primers 5¢-GCAGGTGTGAATTCCATGGTGAGCAAGGGCGAG GAGC-3¢ and 5¢-CCAGATCGCGGCCGCCTTGTACAG CTCGTCATGCCGAGAG-3¢; EcoRI and ApaI restriction enzyme sites were introduced into the 5¢-end and 3¢-end of the Cerulean DNA fragment This DNA fragment was inserted into multiple cloning sites of pEYFP-C1 Venus by EcoRI and ApaI digestion and ligation The resulting vector has Venus followed closely by Cerulean, and between them there are two restriction enzyme sites, BglII and EcoRI, which then were employed to insert the a-helix linker The a-helix linker DNA, 5¢-GGCCTGCGCAAGCGCTTACG

A

C

B

D

Fig 10 Normal expression of stFRET in various host proteins.

a-Actinin–stFRET (A), a-actinin–GFP (B), filamin A–stFRET (C),

filam-in A–CFP (D), spectrfilam-in–stFRET (E) and spectrfilam-in–CFP (F) filam-in 3T3

fibro-blast cells; Collagen-19–stFRET (G) and COL-19–GFP (H) in

C elegans (with assistance of R Gronostajski; Biochemistry

Department, State University of New York at Buffalo, NY, USA).

Arrowheads indicate the striated expression pattern and central line

in the worm cuticle.

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