Journal of Student Research (2013)

Volume 2, Issue 1: pp.

48-51

Research Article

a.Department of Physics, Astronomy and Geophysics, Connecticut College, New London, CT06320

48

The Black Box Module for Low-Level Fluorescence

Detection Targeting Optogenetic Studies

Elizabeth Maret

a

and Mohamed Diagne

a

In optogenetics, genetic labeling by enhanced yellow fluorescent protein (EYFP) indicates transfected neurons expressing light-

gated channel proteins, Channelrhodopsin-2 (ChR2) and Halorhodopsin (NpHR) for millisecond timescale optical manipulation

of neurons.

However, poor spatial understanding of transfection relative to probing is responsible for blind stimulation in

complex mammalian systems and necessitates histological analysis of brain tissue.

Repeatable optogenetic studies on well-

trained and valuable subjects are therefore impossible.

We report here the Black Box Module as a novel fluorescence detection

system targeting EYFP emission and used in conjunction with a co-axial waveguide “optrode.

” Results of the Black Box

Module’s fluorescence detection performance in a bench-top environment simulating EYFP fluorescence with rhodamine 6g are

presented.

We show the Box’s filtration system to be sensitive to the EYFP-like fluorescence of rhodamine and its concentration

dependent emissions behaviors.

We anticipate these results to be the initial foundation in integrating the Box into optogenetic

studies as a tool for locating areas of ChR2 and NpHR transfection.

Keywords: Enhanced Yellow Fluorescent Protein, Black Box Module, Rhodamine 6G, fluorescence

1.0 Introduction

Optogenetics enables cell-type specific targeting and

millisecond timescale control of neuron action potential

events through viral vector transfection of light-responsive

channel proteins.

Light-gated channel proteins

Channelrhodopsin-2 (ChR2) and Halorhodopsin (NpHR) are

conjoined with enhanced yellow fluorescent proteins (EYFPs)

to visually label areas of neuron transfection

[1,2,4,6,8]

. Dual-

function optical stimulation and electrical recording of neuron

action potential events are accomplished through an

“optrode,” a waveguide-based neuroprobe

[10]

.

While the optrode has shown its value as a tool in precise

stimulation and collection of electrical action potentials when

located in an optogenetically transfected areas, locating areas

of transfection remains a challenge

[4]

. This leads to blind

probing, preventing repeatable studies and the possibility of

studies focused on brain layer targeting

[4,11]

. Collection of

fluorescence marking ChR2 and NpHR expressing cells has

initiated a new generation of low-light optical detection for

systems such as one-photon and two-photon fluorescence

microendoscopy and in vivo imaging at the single neuron

level

[3]

. Despite these advances, spatial understanding of

optical probing relative to areas of transfection is limited.

This compromises experimental success and requires

histological analysis of subjects to determine transfection

patterns

[4]

. It is thus both desirable and economic to perform

multiple optogenetic studies on valuable and well-trained test

subjects.

To address this issue, we present the Black Box Module

used in tandem with the optrode, as a novel system to collect

fluorescence from optogenetically modified neurons

exhibiting EYFP expression as is used to label ChR2 and

NpHR in optogenetics.

Using the optrode’s waveguide fiber

core, in addition to its simultaneous optical stimulation and

electrical recording dual-functionality, we believe the optrode

when used with the Black Box Module can also be used for

optical fluorescence collection.

Hence, the optrode-Box

combination can be used to indicate locations of transfection.

We substantiate this prediction by demonstrating how

light collected by the optrode and delivered through its optical

fiber into the Box isolates for EYFP fluorescence and in

addition is sensitive to concentration dependent properties of

rhodamine 6g.

This is achieved through a series of filters

within the light-tight environment of the Black Box.

Highly

filtered fluoresced light is detected by photomultiplier tube

(PMT).

Thus a signal detected by the PMT can verify the

optrode’s position in an optogenetically modified

environment while no signal indicates and non-optogenetic

environment.

Our Black Box system uses free space coupling in a

light-tight environment, opposed to the split fiber

fluorescence detection system of Diester et al (2011)

[4]

. We

believe this to be an improvement over the shared core of the

split waveguide fiber because it allows for increased

opportunities of optical filtration to isolate for fluorescent

light.

We present the results of a study using the Black Box

to detect concentration dependent emissions behavior in a

fabricated bench-top optogenetic environment using

rhodamine 6g fluorescent dye, which mimics EYFP

stimulation and emissions.

The results show the optrode-Box

set up to be sensitive to rhodamine 6g’s concentration

dependent emissions wavelength shift behavior while

maintaining the integrity of its filtration system.

2.0 Experimental Procedure

EYFPs have a quantum yield of 0.

61

[9]

. That means that

in optogenetic environments for every EYFP emission event

there are 64% more laser photons than fluorescence photons.

Hence, key to transfection labeling fluorescence detection is

creating an environment that can isolate detection for

fluorescence.

The Black Box Module (Figure 1) is an 18 in.

x

12 in.

x 7.5 in.

light-tight enclosure made from 3/8 in.

thick

black anodized aluminum plates, containing an optical

filtration system isolating for EYFP emission (525 nm peak)

(Figure 2).

The stimulating laser (Opto Engine), emitting at

473 nm, is fixed within the box and free-space couples to a

Journal of Student Research (2013)

Volume 2, Issue 1: pp.

48-51

Research Article

ISSN: 2167-1907

www.jofsr.

com

49

dichroic beamsplitter (Semrock Brightline FF520-Di02).

Initially, laser light is directed perpendicular from its source

by the beamsplitter and free-space coupled to an optical fiber,

which passes through the wall of the Box to butt-couple with

the optrode.

Laser light then exits the optrode to illuminate a

rhodamine solution and stimulate fluorescence.

Fluorescence,

scattered laser light, and ambient light are collected by the

optrode’s waveguide core to re-enter the Box.

Once inside,

collected light exits the fiber to strike the dichroic mirror at

normal incidence, allowing light above the 520 nm edge

wavelength to pass through.

The collected light then passes

through two identical optical filters (Semrock Brightline

FF01-542/27) with transmission bandwidth 528.

5-555.

5 nm

(Figure 2).

A pin-hole spatial filter controls beam divergence

before incidence on the photomultiplier tube (PMT)

(PerkinElmer MP 942).

The PMT is positioned within the

wall of the Box and an oscilloscope connects to the externally

protruding end.

Figure 1: Black Box Module stimulation and collection

schematic.

The Box’s method of EYFP fluorescence isolation using

optical filters is highlighted in Figure 2, showing the filter’s

transmission bandwidth to isolate for EYFP’s peak emissions

at 525 nm and blocking out laser light at 473 nm.

As

previously stated, initial fluorescence detection as measured

by the Box was performed using rhodamine 6g fluorescent

dye in an ethanol solution to mimic EYFP emissions.

Rhodamine’s stimulation and emissions spectra mimic that of

EYFP’s as shown by the close overlap of spectra in Figure 3.

Figure 2: EYFP absorption and emissions spectrum (blue).

The light green shading highlights the optical filter bandwidth

(542/27 (EM Filter)).

The solid blue line indicates the 473 nm

stimulating laser light (courtesy of Invitrogen Fluorescence

SpectraViewer).

Figure 3: EYFP (blue) and rhodamine 6g (green) absorption

and emissions spectra.

The stimulating laser light is

represented as the solid line at 473 nm.

(Courtesy of

Invitrogen Fluorescence SpectraViewer)

Literature reports rhodamine to exhibit concentration

dependent emissions qualities.

We used the Black Box to

measure fluorescence over a range of concentrations in

attempt to observe the Box’s sensitivity to the concentration

dependent behavior.

Fluorescence response was measured as

photon count events over 1x10

-7

M – 1x10

-2

M rhodamine

concentrations in an ethanol solution by increments of 1x10

-7

M, 5x10

-7

M, 1x10

-6

M, 5x10

-6

M, 1x10

-5

M, and so on until

1x10

-2

M. Thus, fluorescence photon counts were taken at a

total of 11 concentrations.

Fluorescence response was

measured as the frequency of photon count events per second

as recorded by the PMT.

A base noise count of photon events

on the PMT was measured in a 100% ethanol solution

between each fluorescence measurement.

Base noise counts

were directly related to the stimulating laser intensity.

Measurements for the 11 concentrations were taken at four

base count intensities: 1 kHz, 10 kHz, 100 kHz, and 1 MHz.

The relative fluorescence response N relative to the base

count was found by the equation:



N

c

m

c

b

c

b

(1)

where c

m

is the measured fluorescence count and c

b

is the base

count.

Rhodamine exhibits secondary emissions from the

approximately 475-525 nm overlap in its absorption and

emissions spectrum

[5]

. Measuring emissions at wavelengths

outside the area of overlap show low concentrations of

rhodamine to have a constant linear quantum yield in the 1x10

-6

M – 1.5x10

-4

M range

[5]

. Optical filters in the Box isolate for

fluorescence outside the overlap in the 528.

5-555.

5 nm

transmission bandwidth of the filter.

Thus, the Box’s measured

fluorescence response is expected to also exhibit a constant

linear trend until 1.

5x10

-4

M.

As rhodamine concentrations increase to 2x10

-4

M, the

monomer solution forms polymers.

The solution’s change in

composition alters the light interaction with the molecule, and

rhodamine’s emissions spectrum shifts towards infrared

wavelengths as concentration increases

[5,7]

. Kubin and Fletcher

(1982)

[7]

report that at 1.

5x10

-7

M, peak emission occurs at

approximately 525 nm compared to approximately 580 nm

emissions at 1x10

-3

M

[7]

. It must be noted that the Box’s filters

block out wavelengths above 555.

5 nm and Kubin and Fletcher

Journal of Student Research (2013)

Volume 2, Issue 1: pp.

48-51

Research Article

ISSN: 2167-1907

www.jofsr.

com

50

cite no upper limit to the concentration dependent red shift

behavior.

Therefore, as rhodamine concentrations increase and

the fluorescence emissions redshifts, the Box’s measured

response rate is expected to slow and show a decrease in

response as it reaches concentrations exceeding 1x10

-3

M.

Based on the properties of rhodamine described above there

are two key properties the Box’s sensitivity must accommodate

to be considered for optogenetic environments.

First, it must

pick up on the low concentration linear quantum yield to verify

its sensitivity to fluorescence detection.

Second, due to

rhodamine’s red-shift under increasing concentrations, the Box’s

measurements must show a decline in count rates at

concentrations beyond 2x10

-4

M to claim the validity of the

optical filters.

3.0 Results

3.1 Rhodamine Redshift

Data collectedover the 1 kHz, 10 kHz, 100 kHz and

1MHz base counts are shown in Figure 4.

Responses across

the 1 kHz, 10 kHz and 100 kHz base counts show the relative

response rate to notably slow between 1x10

-3

M and 5x10

-3

M.

Responses for the 1 MHz base count saturated the

sensitivity parameters of the PMT at concentrations above

1x10

-5

M and hence Figure 4 shows no fluorescence response

for concentrations above 1x10

-5

M.

Figure 4: Rhodamine’s relative fluorescence response for 1

kHz, 10 kHz, 100 kHz, and 1 MHz base counts of 1x10

-7

– 10

-

3

M concentrations.

3.2 Low-Concentration Constant Quantum Yield

Examining the 1 kHz base count behavior, Figure 5

shows the constant quantum yield behavior as measured by

the Box for the 1x10

-7

– 1x10

-4

M concentration range.

This

behavior is similarly observed at the 10 kHz, 100 kHz and 1

MHz base counts (not presented here).

Figure 5: Rhodamine’s low-concentration constant quantum

yield for 1 kHz base count.

4.0 Discussion

As expressed in Section 3.

1, Figure 4 presents

rhodamine’s relative response across all base counts.

Within

the 1x10

-3

M and 5x10

-3

M concentration range, the 1 kHz, 10

kHz and 100 kHz base counts show the response rate to slow.

This range corresponds to the region in which Kubin and

Fletcher (1982)

[7]

report a value of approximately 580 nm for

rhodamine peak emissions, which lies outside the

transmission bandwidth of the Box’s filters.

Moreover,

Figure 4 shows that within this range the fluorescent response

rate decreases between 5x10

-3

M and 1x10

-2

M. Since Kubin

and Fletcher do not cite an upper limit in rhodamine’s red

shift behavior, we believe the red shift behavior continues

such that the peak emissions wavelength shifts further outside

the filters’ transmission bandwidth.

Thus, as concentration

increases beyond 1x10

-3

M, more fluorescence is filtered out,

causing a decrease in detection by the PMT.

Section 3.

2 described the Box’s detection of rhodamine’s

low-concentration behavior.

The linear trend of the data

confirms rhodamine’s expected constant quantum yield at

concentrations below 2x10

-4

M, as expressed by Fischer and

Georges (1996)

[5]

.

The Box’s sensitivity to the concentration dependent

redshift and constant low-concentration linear behavior of

rhodamine confirms its ability to isolate for EYFP-like

fluorescence.

This presents the prospect of addressing the

explicit concern of Diester et al (2011)

[4]

in the need for

improved spatial understanding of optogenetic probing to

locate areas of transfection.

Considering that EYFP peak

emissions is understood to be constant compared to

rhodamine’s concentration emissions, we expect the Box’s

filtration and detection system to be able to separate and

detect EYFP fluorescence from scattering laser and noise light

signals.

To verify this, the next step is to use the Black Box

to measure actual EYFP fluorescence.

Provided this next

study is successful, we predict the Box-optrode system can

eventually be used to locate areas of Chr2- or NpHR-EYFP

expressing neurons indicated by collecting positive

fluorescence signals.

Journal of Student Research (2013)

Volume 2, Issue 1: pp.

48-51

Research Article

ISSN: 2167-1907

www.jofsr.

com

51

Before the Box-optrode system is regularly integrated

into optogenetic studies it is necessary to calibrate the system

for areas of transfection.

The potency of viral vector

transfection and how it spreads through a volume is still under

examination

[4]

. Thus it is important to examine the event

count signatures associated with differing EYFP potencies as

a further means of achieving spatial understanding when

probing.

5.0 Conclusion

By the ability of the Box’s low-level fluorescence

detection system used with the optrode to detect expected

behaviors in rhodamine’s concentration dependent

fluorescence response, we are confident in its function as a

tool for fluorescence detection.

This study also displays the

optrode-Box combination has the potential to jointly achieve

optical stimulation, optical and electrical recording.

We

anticipate the Box’s integration into in vivo optogenetic

studies to improve spatial understanding in optogenetic

probing and significantly reduce the need for terminal

histological analysis on expensive test subjects.

Acknowledgements

This work was supported by the Defense Advanced Research

Projects Agency (Repair Program) subcontract no.

25480040-

47135-B, and a startup fund from the Dean of Faculty Office

at Connecticut College.

The authors would like to extend their

sincere gratitude and appreciation to Professor Arto

Nurmikko of Brown University and his team for this

incredible undergraduate research opportunity.

Thanks to

Ilker Ozden and Jing Wang from Brown University for their

contribution in optimizing the module performance.

Role of the Funding Source

This work was supported by the Defense Advanced Research

Projects Agency (Repair Program) subcontract no.

25480040-

47135-B, and funds from the Dean of Faculty Office at

Connecticut College.

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