Single Molecule Detection (SMD)

Single Molecule Incentive

The ultimate limit to analytical sensitivity is the reliable detection of single molecules. Recent technical advances in optical detection and manipulation have made the detection of isolated, light emitting probe molecules a reality. Thus we are witnessing a burgeoning interest in the imaging and spectroscopy of single molecules, particularly within the fields of cell biology and drug discovery.

Of particular importance to biology is the possibility of direct, real-time visualization of single biological macromolecules and their assemblies under native physiological conditions, offering great promise for enhancing our understanding of the behaviour, interactions and trafficking of individual biological macromolecules within the living cell. Such studies have increased medical and pharmaceutical significance within the developing post-genomic era of proteomics, providing the means to track the behaviour and mechanistic involvement of biochemically relevant single proteins.

It is reasonable to ask why it is interesting to observe the emission from a single fluorophore, since numerous fluorophore labels can be detected within a diffraction-limited spot. There was a time when the scientific community was content with detecting the combined signal of a vast number of fluorescent (or Raman active) molecules from a point of interest within the sample. There is a rapidly growing realization however, particularly within the life science and materials science fields, that the information content afforded by imaging the single fluorophore markedly exceeds that offered by the "bulk" ensemble measurement, yielding invaluable insight into individual molecular properties and their micro-environment.

Experiments on single molecules have attracted vivid interest in many branches of fundamental research because they allow for the study of molecular properties normally disguised in inhomogeneous distributions of an ensemble. In contrast to observing the position of several labelled molecules at a given position, single molecule detection provides additional information, such as:

  • Polarization or image spot shapes indicate orientation and reorientation.
  • Time traces of intensity, emission spectrum, or fluorescence lifetime provide information on local dynamics and diffusion.
  • Fluorescence Resonance Energy Transfer (FRET) provides information on the proximity of specific labelled sites less than 10nm apart.
  • Position sensitivity allows an investigator to locate a molecule and follow simultaneously the translational motion, re-orientational motion, and the internal dynamics of the individual molecules.

Single molecule studies are uniquely poised to yield information about molecular motion, behaviour, and fluctuations over time and space. There are many biological molecules that can avail from examination at this level, typical subjects being key members of a system that are receptive to specific cellular signals, environmental perturbations or drug intervention. Cellular mechanisms that have been examined include ion channel activity, protein folding, enzyme activity, membrane structure, molecular motors/motility and vesicle transport. Single molecule detection is a way to study detailed physical and chemical properties that allows for scrutiny of fundamental principles and mechanisms, and may lead to technological and methodological developments.

Single molecule techniques also have key potential in material development. The single molecule is an excellent probe of local (nanoscale) properties since it is a quantum light source with spectrum and lifetime that is sensitive to its chemical and physical environment. The rotational and translational motion of single molecules can be measured and used to understand the local mechanical properties of the material in which the molecules are embedded. Thus groups are seeking to understand and catalogue the great variety of behaviours of single molecules in technologically relevant environments to better use these probes to study the small-scale structure.

Parallel Detection by Camera

One of the compelling aspects of single molecule studies is the ability to directly observe distributions of individual properties and molecular behaviour. Obtaining distributions of such parameters requires studying a large number of individual molecules. Single molecule microscopy using camera detection has the capability to effectively investigate many spatially separated individual molecules in a parallel fashion.

Such an approach can make for more efficient experiments and ensure that the molecules are imaged under identical conditions. Specific statistical distributions of properties can be determined which contain more detailed information than the ensemble-averaged mean values obtainable by bulk measurements.

From an analytical perspective, single molecule measurements have ultimate sensitivity, opening a new era of femtomolar chemistry, by which biological reactions and high-throughput screening can be carried out with minute samples, which are normally insufficient for measurement purposes.

One area of particular commercial vibrancy is the drive towards extremely efficient whole genome sequencing using single molecule approaches. The ultimate goal here is to make available the capability to screen the entire 3 billion bases of the human genome within 24 hours, for less than $1000!

Camera-Based SMD Techniques

The continually improving technologies of modern lasers, ultrasensitive detectors, analysis software and novel optical configurations, permit detection and investigation of single molecule fluorescence images, trajectories, spectra, and lifetimes.

Some of the camera-based techniques adaptable to single molecule detection are listed below, their suitability depending more on the specific system under study:

  • Confocal Raman Microscopy
  • HyperSpectral Imaging
  • Spinning Disk Confocal Laser Scanning Microscopy
  • Total Internal Reflectance Fluorescence Microscopy (TIRFM)
  • Widefield Epifluorescence Microscopy

Background Photon Noise - The Need to Minimize

Background photon noise level must be low compared to the signal level in order to allow discrimination of single molecules. This is usually the most serious limitation to sensitive detection. Just as stars can be seen at night but are obscured by sunlight scattered from our atmosphere during the day, the key to SMD is to minimize background, which includes fluorescence or Rayleigh/Raman scattering of the bulk medium containing the molecule of interest.

This is normally realized by some combination of spectral, temporal or spatial filtering. Spatial discrimination, has the effect of increasing the apparent concentration of the molecule of interest - one molecule confined to a 1μL and a 1fL volume has effective concentrations of 10-18 M and 10-9M respectively.

The proportion of the total signal that originates from the molecule can thus be increased significantly by miniaturization. Spatial discrimination also helps to isolate single molecules, as the probability of finding more than one molecule in the same volume element (for a given bulk concentration) decreases with a decreasing volume.


TIRFM

A relatively straightforward way to limit the observation volume is to excite the molecules by Total Internal Reflection (TIR) illumination. TIRFM makes use of an optical effect that can be adapted to observe fluorescent events occurring at the interface between two optical media of different refractive indices. Excitation light incident upon such a boundary, travelling at an angle greater than the critical angle, undergoes total reflection.

The electromagnetic field of the total internal reflected light extends into the sample beyond the interface, extending only a few hundred nanometres into the second medium of lower refractive index - essentially in the z direction. Furthermore, this Evanescent Field decreases exponentially in intensity along the z-axis of penetration. Only the section of the specimen located within the evanescent field undergoes fluorescence excitation.

TIRFM is limited to the area within a few hundred nanometres of the glass/sample interface, where total internal reflection is occurring. By imaging the surface onto a camera, individual molecules can be registered as each migrates to the proximity of the surface. This imaging method allows the observation of many distinct molecules simultaneously, yielding a high throughput and increased statistical viability.

TIRFM is an increasingly popular technique for visualizing, with high signal to background ratio, single molecule processes that occur in and around the membrane of living cells (partially due to availability of novel membrane-specific fluorophores). In contrast to the spinning disk confocal technique, which can yield rapid optical sections of approx. 1μm thickness, the excitation volume of a TIRF evanescence field extends only approx. 100nm into the sample, the intensity of which decays exponentially across this distance. Since only a very thin sliver of excitation is being produced, we only detect photons that are created within that excitation volume, which has the effect of significantly improving signal to background.

Whilst a thin excitation volume of the order of 100nm depth sounds very useful, it must be remembered that due to the nature of the TIRF effect, we cannot step this excitation plane through the volume of the cell. TIRFM is a surface interface phenomenon, and as such is restricted to studying sample that is within 100nm or so of the glass interface of the slide. For events within the bulk volume of the cell, we must rely on widefield epifluorescent or a rapid confocal scanning approach.

Multiple Probes and FRET

It is often of interest to dynamically image multiple different biomolecules, and their interactions within the sample volume. The TIRFM technique can readily be extended to image multiple fluorophores labels, through integration of a multi-line laser system, preferably a solid-state laser solution with Acousto-Optical Tunable Filter (AOTF) modulation.

This technique can be readily adapted for FRET analysis, preferably through integration of a suitable beam splitting device on the emission side.

Electron Multiplying CCD (EMCCD) - the Last word in Ultra-Sensitivity

EMCCD technology is the ideal detector for dynamic single molecule imaging. The extraordinary Signal to Noise (S/N) offered is significantly greater than that afforded by conventional CCD cameras operated at fast readout speeds. EMCCDs exhibit frame rates that are ideally suited to dynamic acquisition of transient single molecules and their interactions. Since EMCCDs are array detectors, multiple single molecules can be illuminated and imaged in parallel, greatly improving the experimental throughput and statistical viability of SM data.

Underlying all direct imaging studies of living cells or organisms, is the desire to preserve the living subject for as long as possible, through minimization of both phototoxic cell/tissue damage and also photobleaching of the incorporated fluorophores. As such, techniques for studying single molecules benefit markedly from using EMCCD detection technology, permitting the laser or lamp excitation light to be attenuated.

The spectral properties of single molecule systems can be accessed in a number of ways. For example, simply through fast switching between multiple fluorophores excitation/emission, or even splitting of the emission signal simultaneously onto different areas of the sensor. Through minimization of excitation powers, the rates of dye photobleaching and cell phototoxicity are significantly reduced.

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