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Research Papers

CamesanoAbuLailBiomacromol2002

bacterial surface (with polymers that range in size from tens to hundreds of nanometers and have adhesion affinities for the AFM tip from 0-1nN)

adhesion between bacteria and surfaces is important for environmental and biomedical applications such as in situ bioremediation, microbially facilitated transport of contaminants and biofilm formation on biomaterials and implants

bacterial adhesion depends on polymers on the surface, but prediction of attachment based on biopolymer properties are not possible

sample prep:

bacterial cells bonded to glass slides (ref. 33)

hydrated

experiment in  pure water, 0.01M-0.1M KCl

AFM:

DI Dimension 3100 with Nanoscope III controller

silicon nitride tips (DNPS) from DI

CarrionVazquezProgBiophysMolBio

review

Invention of AFM: Binnig et al., 1986

Imaging most frequent application

Force spectroscopy mode of AFM was developed later (Burnham and Colton, 1989) and applied to receptor-ligand systems (Florin et al., 1994, Science 264, 415-417.)

advantages: few micrograms of protein needed, no size limitation, no crystals needed 

review mostly on AFM to study the molecular determinants of the mechanical stability of proteins

comparison of alpha-helical and beta-sheet proteins

(un)folding of mechanical proteins

examples of proteins that are exposed to mechanical tension: titin, extracellular matrix proteins, cytoskeletal proteins

one structural characteristic common to proteins exposed to mechanical tension is that they contain multiple individually folded domains

domain architecture

references to other reviews of AFM

FisherNatureStructBio2000

Review

saw-tooth pattern of force peaks is the unmistakable fingerprint of a modular protein

each peak corresponds to the consecutive unfolding of each of the protein domains in a single molecule

can yield unfolding force peaks equal to the number of domains in the protein, but more frequently will yield fewer peaks or no peaks at all

spacing between the peaks reflects the number of amino acids that each unfolding event adds to the total length

molecular dynamics simulations suggest that force=induced unfolding occurs through different pathway than chemical unfolding

FotiadisMicron2002

GouauxWhiteCurrOpinStructBio2001

GroganBiosensorsBioelectronics2002

AFM and biosensor: development of cantilever-based immunosensors

Definition of biosensor: Biosensors are analytical devices which combine a biologically sensitive element with a physical or chemical transducer to selectively and quantiatively detect the presence of specific compounds in a given external environment (ref. Nicolini et al, 1992)

Applications: diagnostic and therapeutic monitoring in clinical applications (frequent testing with short turnaround times)

Get review for microfabtricated cantilevers to use in bio-chemical sensing: Raiteri and Grattarola (2001)  in Sensors and Actuators B.

antibody is the sensing element, microcantilever acts as a mechanical transducer

measure the activity, stability, lifetime and reusability of antibodies to myoglobin covalently immobilized onto microfabricated cantilever surfaces: stable for up to 7 weeks

next stage: use an array of cantilevers - the net differential signal from the array of cantilevers is the sensor signal (get ref. Fritz et al. (2000) Science 288, 316-318.)

major challenges in biosensor design: reproducibility, long term drift of cantilever bending, understanding of the mechanism of binding of analyte to the cantilever surface

use two cantilevers: one as reference, one as sample, can improve the sensitivity

AFM:

silicon nitride (DI)

flowing cell

Sample prep:

Cantilever surface: first, sulfo-LC-SPDP from Pierce react with antibody NH2, plus DTT to reduce SS to SH, then self-assembly on gold surface

 

HasegawaBiochem2002

amyloid fibrils

sample prep:

C1 sensor chip (BIAcore) in which the carboxymethyl residue was directly coupled to the gold thin layer with no dextran chain 

coupling done within the BIAcore flow cell, then take it out, remove the glass support from the plastic support by dissolving the adhesives with ice-cold acetone

AFM:

dynamic force microscope SPI-3800N-SPA400

scanning microcantilever (SI-DF20) (Seiko Instruments)

HeymannJStructBiol1999

comparison of X-ray diffraction, electron crystallography and AFM 

AFM particularly useful to study the surface properties and dynamics

HeymannStructureFoldDes2000

rhodopsin loop grafted onto br

different salt concentration was necessary than was used with normal br

standard deviation map useful for study of flexible loops

AFM is not able to image segments that are really unstructured

Sample prep:

purple membrane was diluted to 10mg/ml in 300mM KCl pH 7.8, 10mM Tris-HCl prior to adsorption (ref. Mueller and Engel (1997) Biophys. J. 73, 1633-1644.

20 min adsorption

washing gently with imaging buffer: 10mM Tris-HCl, pH 7.8, 100-150mM KCl

HugelScience2002

light-powered molecular machines are probably essential constituents of future nanoscale devices

new development: optically lengthen and contract individual polymers by switching the azo groups between trans/cis configs.

polymer contracts against an external force acting along the polymer backbone, thus delivering mechanical work

Optomechanical energy conversion in a single-molecule device

 

LeckbandCurrOpinStructBio2001

MoellerJMB2000

Bacteriorhodopsin

after photobleaching in presence of hydroxylamine: loss of crystalline properties, but br is still a trimer

note on comparison to rhodopsin

Sample prep:

before use, the fluid cell was cleaned with conventional dish cleaner

rinsed with ultra pure water and ethanol

muscovite mica was punched to 6 mm diameter and glued onto 12 mm Teflon disc with water-insoluble epoxy glue

Mica New York Corp., New York, USA:    

1412-T W. Broadway
New York , NY 10018

Tel: 212-354-2664
Fax: 212-354-2860

teflon disc glued onto a slightly smaller steel disc to allow magnetic fixing of the sample on to the piezo scanner

MooreEMBO2001

MuellerBBA2000

Review

resolution of AFM ~0.5nm

imaging of a statistically significant number of single proteins by AFM allows their structural variability to be assessed

determine the principal modes of protein motion

observe directly conformational changes of single proteins and of their assemblies

conformation changes can be induced in a controlled manner to identify flexible protein structures

Review of br results

MuellerJMB1995

Bacteriorhodopsin:

purple membranes at 50 mg/ml suspended in 150 mM KCl, 10mM Tris, pH 9.2

Sample preparation:

purple membrane suspension 50mg/ml was absorbed to freshly cleaved mica for 30 min

wash to remove not absorbed material

AFM:

Nanoscope III (Digital Instruments, CA)

15mm or 130mm piezo scanner 

oxide sharpened silicon nitride tips mounted on a 100mm cantilever (Olympus Ltd. Tokyo, Japan)

SEMPER image processing system (Saxton et al., 1979)

MuellerJMB1999

Bacteriorhodopsin:

purple membranes isolated from Halobacterium salinarum ET1001 according to Oesterhelt and Stoeckenius, 1974

orthorhombic 2D crystals prepared as described by Michel et al, 1980

Sample preparation:

adsorbed onto freshly cleaved mica in buffer 300mM KCl, 10mM Tris-HCl, pH 7.8 according to Mueller, Amrein and Engel (1997) Adsorption of biological molecules to a solid support for scanning probe microscopy. J. Struct. Biol. 119, 172-188.

Experimental Conditions:

100mM KCl, 10mM Tris-HCl, pH 7.8

AFM:

Nanoscope III (DI) with E-scanner (12mm) and oxide sharpened Si3N4 tips on a cantilever with a spring constant of 0.1N/m (Olympus)

OesterheltScience2000

Bacteriorhodopsin:

- purple membranes of H. salinarum strain S1 isolated as described in Oesterhelt and Stoeckenius, Methods Enzymol. 31, 667 (1974).

- stock solution of protein (5 mg/ml) in ultrapure water at 4oC

AFM:

Nanoscope III (Digital Instruments, Santa Barbara, CA) equipped with a J-scanner (80mm) and oxide-sharpened Si3N4 tips on a cantilever (Olympus, Tokyo)

spring constant of cantilever as estimated by analysis of the thermal noise spectra 0.1N/m

Experimental Conditions:

300mM KCl, 10mM Tris-HCl, pH 7.8

RT

Experiment:

position the tip, apply force to absorb protein on stylus and pull out

 

Reference in Forbes and Lorimer commentary: use AFM to study folding and MISFOLDING: Oberhauser et al. (1999) Nature Struct Biol. 6, 1025

OuerghiBiomolEng2002

antigen-antibody immune complex

Sample preparation:

antibodies in PBS at a few mg/ml

deposit on freshly cleaved mica surface for 15 min at RT

rinse with deionized water to remove salts and weakly adsorbed antibodies

dry under Nitrogen

for binding of antigen: surface was exposed to buffer with antigens in same way as for antibodies

References for different substrates for flat solid surface immobilization: silicon oxide, gold, mica, polystyrene etc. , native and modified mica are the most commonly used

Experimental conditions

air, RT

AFM

Nanoscope IIIa (DI)

in non contact (tapping) mode and multi channel data acquisition

silicon lever

ParbhuBiochem1999

keratin fibers

Experiment: 

imaging AND indentation

AFM imaging:

multimode AFM with J-scanner and Nanoscope IIIa controller (DI)

imaging in tapping mode in air with 125mm etched silicon microcantilevers (TESP)

AFM indentation:

diamond tip cantilever (DI)

tip was a single crystal of natural diamond bonded with epoxy to the stainless steel cantilever

Sample prep:

slices cut were mounted on 100 mesh Formvar-coated PELCO copper locator grids where each mesh point is uniquely identified

 

PereiraBiochemPharm2001

RiefJMB1999

spectrin

unfolding

Monte Carlo simulations

picoNewton

Sample prep:

spectrin from Sigma

adsorb onto a freshly evaporated gold surface or a freshly cleaved mica surface from a 50 ml drop of the solution for 10min

rinse with PBS

measure in PBS

AFM

homebuilt

silicon nitride cantilevers (Park Scientific, Stanford) were used as force sensors

RiefScience1999

picoNewton instrumentation

dextran

MD calculations

Sample prep:

dextrans linked to gold surface through epoxy-alkanethiols, activated with one carboxymethylgroup per glucose, reacted with streptavidin so that they can be bound to Sensor chip SA5, Pharmacia Biosensor AB, Uppsala, Sweden

AFM cantilever with biotin bound to the AFM tip was used to pull the dextran through the biotin-streptavidin bond

all measurements in PBS

cantilevers were silanized in deimethyl-dichlorosilane (Sigma) vapor and rinsed with acetone

commercially available carboxymethylated dextran films on gold (Sensor Chip CM5, Pharmacia), Pharmacia Biosensor AB, Upppsala, Sweden) were used as samples

AFM:

homebuilt AFM

cantilevers (DI)

RuanAnalChem2002

biosensor application of AFM: detect change in surface characteristics of E. coli before and after binding of antibodies

biosensor can detect with limit 6000 cells/ml

previous detection methods: 

    1. quartz crystal microbalance as the electronic transfer means for binding event

    2. surface plasmon resonance

    3. electrochemical impedance

Challenge in immunosensor development: signal amplification of the binding event

AFM:

Nanoscope IIIa (DI) in tapping mode

Sample prep:

ITO-coated glass (CG-80IN-1515) was purchased from Delta Technologies (Stillwater, MN) was cut into 5x0.8cm slices

clean with acetone, ethanol, water

10 min 1M HCl

wash with water

1:1:5 (v/v) H2O2/NH4OH/H2O for 1 h

rinse with water

before the silanization, the chips were dried under a stream of nitrogen

etc., also see previous ref. 19

after silanization the surface had many exposed active epoxy groups that react readily with protein amino groups

anti-E coli antibodies in drop 5 ml of 1mg/ml antibody onto substrate chip (8mmx8mm) 24 h at 4oC

middle part of the ITO chips was coated with 5-min Epoxy to avoid contact with the solution

antibody chips were rinsed with water and incubated with 50 ml of heat-killed E. coli (10000-70000 cells/ml) for 1 h at 37oC)

 

ZlatanovaProgBiophysMolBio2000

excellent review!!

what forces govern specific molecular interactions? they result from multiple weak, non-covalent bonds

how to probe such weak interactions?

    1. surface force apparatus

    2. pipette suction

    3. magnetic beads

    4. flow chamber apparatus

    5. optical traps and tweezers

 

 

 

 

© 2002 Judith Klein-Seetharaman, University of Pittsburgh. This website was created December 12, 2002 and updated January 21, 2003. For questions or comments please contact Judith Klein-Seetharaman at jks33@pitt.edu.