IN SITU HYBRIDIZATION OF NON-RADIOLABELED RNA PROBES TO SECTIONED TISSUE.

 

 In situ hybridization is a useful technique for determining spatial patterns of gene expression.  In this lab, we will carry out hybridizations of digoxigenin labeled probes to plant material that has been fixed, embedded in paraffin, sectioned and placed on microscope slides.  We don’t have enough time to carry out the entire protocol - it takes a week just to fix and embed tissue - so we will perform only the actual hybridization.  You will be provided with slides that have sectioned siliques on them.  The siliques, and the embryos within them, are at various stages of development.  You will also be provided with probes for transcripts that are localized to specific subdomains of the developing embryo.  (Protocols for tissue fixation, embedding, sectioning and probe synthesis are included for your general information.  These follow the protocols for the hybridization procedure.)

 

The hybridization experiment takes two days.  On the first day, the tissue sections are subjected to a variety of pretreatments and the hybridizations are set up.  On the second day, the tissue sections are washed and the probe is visualized.  The digoxigenin labeled hybrids are detected by applying anti-digoxigenin antibodies to the tissues.  This antibody is conjugated to alkaline phosphatase.  Alkaline phosphatase carries out a reaction that yields a colored (blue in this case) precipitate.  The color develops over the course of one to three days.

 

This protocol is the one used in the Barton lab.  It has been modified by Jeff Long from protocols used in Sarah Hake’s, Vivian Irish’s and Elliot Meyerowitz’s labs.  Useful references for in situ  hybridization to plant tissues are:

 

Jackson, D. (1991) In-situ  hybridization in plants. in Molecular Plant Pathology: A Practical Approach  Eds. Bowles, D.J., Gurr, S.J and McPherson, M.  Oxford University Press.

 

In situ hybridization : a practical approach (1992), edited by D.G. Wilkinson, Oxford University Press.

 

I. TISSUE FIXATION AND EMBEDDING

 

This protocol uses a paraformaldehyde fixative.  FAA (50% ethanol, 5% acetic acid, 3.7% formaldehyde) is an alternative fixative.  (If FAA is used, ethanol series for dehydration begins at 50%.) 

 

Day 1- fix tissue

 

Make up the amount of 1X PBS you will need and adjust the pH to 11 with NaOH.  Heat the solution to 60 to 70°C.  Add paraformaldehyde.  Do this in a fume hood.  The paraformaldehyde should dissolve within a few minutes.  Place solution on ice and when it has cooled to about 4°C, adjust the pH with H2SO4.

 

Dispense the paraformaldehyde solution into glass scintillation vials.  Place vials on ice in a vacuum desiccator.  Add freshly harvested tissue to the vials.  Close the desiccator and apply a vacuum to the samples until the paraformaldehyde solution starts to bubble.  Hold the vacuum for 15 minutes and then release it slowly.  Repeat this procedure until the tissue sinks.  Replace the paraformaldehyde solution with fresh paraformaldehyde solution and shake gently overnight at 4°C.

 

 


Day 2 - dehydrate tissue

 

All steps are done at 4°C with gentle shaking or rotating.  A Labquake rotator works well.

 

 

Solution

 

 

time

 

number of changes

1 X PBS

 

30 minutes

two

30% ethanol

 

60 minutes

one

40% ethanol

 

60 minutes

one

50% ethanol

 

60 minutes

one

60% ethanol

 

60 minutes

one

**70% ethanol

 

60 minutes

one

85% ethanol

 

60 minutes

one

95% ethanol + eosin*

overnight

one

 

*The amount of eosin added is not exact.  Add enough to give the ethanol a nice bright orange color.  The eosin is added to dye the tissue so that it can be easily seen when embedded in paraffin.

 

**Tissue can be stored in 70% ethanol at 4°C for at least several months.

 


Day 3 - Finish dehydration and begin embedding

 

All steps are done at room temperature with gentle shaking or rotating.

 

Solution

time

number of changes

100% ethanol + eosin

 

30 minutes

two

100% ethanol + eosin

 

60 minutes

two

25% Histoclear, 75% ethanol

 

60 minutes

one

50% Histoclear, 50% ethanol

 

60 minutes

one

75% Histoclear, 25% ethanol

 

60 minutes

one

100% Histoclear

 

60 minutes

two

100% Histoclear + 1/4 volume Paraplast Plus (paraffin) chips

overnight

(no shaking)

 

 

 

 

Day 4 - continue embedding

 

Place the vials at 42°C until the Paraplast chips melt completely.

 

Add another 1/4 volume of chips and wait until completely melted.

 

Move vials to 60°C.

 

After several hours, replace the wax/Histoclear solution with freshly melted wax.  Leave overnight.

 

Day 5 - more embedding

 

Replace old wax with fresh wax twice.

 

Day 6 - more embedding

 

Replace old wax with fresh wax twice.

 

Day 7 - more embedding

 

Replace old wax with fresh wax twice.

 

Day 8 - place tissue in molds

 

Place tissue in molds.  We use aluminum weigh boats (Fisher Scientific).  Be careful to arrange tissue in the weigh boats so that it will be easy to cut the wax block into appropriate sized pieces and so that it will be easy to orient the tissue for sectioning.  Store paraffin blocks with embedded tissue at 4°C.

 

 

 


II. SECTIONING

 

Use ProbeOn Plus slides (Fisher Scientific).  They are pre-cleaned, charged, and easily sandwiched together for later steps.

 

Place slide on a slide warmer that has been pre-warmed to 42°C.  Apply several drops of DEPC-treated water to the slide.

 

Cut six to eight micrometer thick sections on a microtome.  Float the ribbons of tissues on top of the water droplet on the slide.  Within a few minutes, the ribbons should flatten out.  Paint brushes can be used to manipulate the ribbons.

 

Wick off excess water from the slide with a Kimwipe.  Excess water can cause the tissue to bubble.

 

Incubate the slides on the slide warmer overnight so that tissue adheres tightly to the slide.  Slides can be stored with desiccant for several weeks at 4°C.

 

 

 


III. PROBE SYNTHESIS

 

Transcription

 

Template:  Transcripts are made from plasmids carrying promoters for T3, T7 or SP6 polymerases.  The plasmid is linearized first.  Be sure to digest to completion.  Do not use enzymes that leave a 3’ overhang.  Phenol/chloroform extract to get rid of any RNAses.  Resuspend the DNA in DEPC-treated water to a concentration of 0.5 micrograms/microliter. 

 

Transcription Reaction:

 

template DNA (0.5micrograms/microliter)

 

4 microliters

5X transcription buffer

(Stratagene)

5 microliters

5X nucleotides

(2.5 mM each;

UTP is 1/2 “cold” UTP and

1/2 dig-UTP (Boehringer,

cat#1209256)

5 microliters

RNASIN (Promega)

(RNAse inhibitor)

to 1 unit/microliter

RNA polymerase

to 0.4 units/microliter

water

 

to total

Total Volume

25 microliters

 

Incubate the reaction at 37°C for 30 to 60 minutes.

 

To check that you have synthesized transcripts, run 1 microliter of transcription reaction on a minigel (add ethidium bromide to gel) at about 100 V for about 15 minutes. The RNA degrades quickly so do not run it for too long.  Treat the gel box and comb with 0.2 N NaOH for 30 minutes before use.  Probe will appear as a band below the template band.  Use the relative intensity of the two bands to estimate the amount of probe synthesized.  If, for instance, the transcript band and the template band are of equal intensity, estimate that you have synthesized 2 micrograms of RNA.

 

Add 75 microliters water and 1 microliter of 100mg/ml tRNA and 5 units of RNAse-free DNAse to transcription reaction.  Incubate for 10 minutes at 37°C.

 

Precipitate RNA probe by adding an equal volume of 4M NH4OAc and 2 volumes of 100% ethanol.  Place at -20°C for twenty minutes. Centrifuge in a microfuge to bring down the precipitated RNA.  Rinse the pellet with 70% ethanol.  Air dry pellet or place tube in speed vac with no heat.

 

 

Carbonate hydrolysis

 

The probe is hydrolyzed into fragments between 75 and 150 base pairs long.  To calculate the length of time to let the reaction go, use the following formula:

 

T (time) = (Li-Lf)/K Li Lf

 

where Li is the initial length of probe, Lf is the final length of probe and K=0.11 kb/minute.

 

Resuspend the RNA pellet in 100 microliters water.  Add 100 microliters 2X carbonate buffer (80 mM NaHCO3, 120 mM Na2CO3).  Incubate at 60°C for the time calculated.  Neutralize with 10 microliters 10% acetic acid.

 

Precipitate with 1/10 volume 3 M NaOAc (pH 5.2) and 2 volumes ethanol.  Place tube at -20°C for twenty minutes, centrifuge and rinse pellet with 70% ethanol.  Resuspend in 50% formamide at a concentration of 1 microliter/slide (see below).

 

The probe is used at a final concentration of 0.5 ng/ microliter/ kb probe complexity.  Hybridizations are done in 100 microliters per slide.  So if your probe is 1 kb, you will need 0.5 ng x 100 microliters x 1 kb = 50 ng of probe per slide.  If your probe is 2 kb, you will need 100 ng of probe per slide, etc.

 

Experiment with different amounts of probe (try up to 5X higher and lower) to find the concentration that gives the best signal. 

 

 


IV. IN SITU HYBRIDIZATION TO SECTIONS

 

DAY ONE

A.  Section Pretreatment

The paraffin is removed from the sections with Histoclear (National Diagnostics) or Citra-Solv (Fisher) and the sections are rehydrated through an ethanol series. 

 

(A note about solutions:  All solutions should be made RNAse free.  Most of the solutions are not diethylpyrocarbonate (DEPC)-treated but everything is autoclaved before use.  Plastic containers are treated with 0.1 M NaOH overnight and rinsed with sterile water.  Be careful to handle all tissue and solutions with gloves to avoid contamination with RNAses.)

 

1.  Deparaffinize and rehydrate sections.  All steps are at room temperature unless otherwise noted.  Place slides in rack.  Move slide rack through the following solutions:

 

Solution

time

number of changes

100% Histoclear

 

10 minutes

two

100% ethanol

 

1-2 minutes

two

95% ethanol

 

1-2 minutes

one

90% ethanol

 

1-2 minutes

one

80% ethanol

 

1-2 minutes

one

60 % ethanol

 

1-2 minutes

one

30 % ethanol

 

1-2 minutes

one

water

 

1-2 minutes

one

2XSSC

 

15-20 minutes

one

 

2.  Protease.  Tissue sections are proteased to increase the accessibility of the target RNA.  Treat sections with proteinase K (1 microgram/ml in 100 mM Tris (pH 8) and 50mM EDTA) at 37°C for 30 minutes.  To make protease solution, prewarm Tris/EDTA solution to 37°C;  then add the proteinase K (from a 10mg/ml frozen stock) immediately before adding slides.

 

3.  “Refix” tissue.  This prevents disintegration of the tissue following protease treatment.

 

Solution

time

number of changes

2mg/ml glycine in

1 X PBS

 

2 minutes

one

1 X PBS

 

2 minutes

two

4% paraformaldehyde, pH 7

(made fresh*)

10 minutes

one

1 X PBS

 

5 minutes

two

 

*See section on fixation for paraformaldehyde recipe.

 

4.  Acetic anhydride treatment.  In this step, positively charged amino groups are acetylated.  This reduces non-specific binding of the probe.

 

Place slides in a solution of 0.1 M triethanolamine (pH 8, made fresh) and acetic anhydride for 10 minutes with stirring.  (To do this, elevate the slide rack above a stir bar).  Dispense the acetic anhydride (4 mls for 800 mls of triethanolamine) into the triethanolamine and mix for a few minutes before putting the slide rack in.

 


5.  Wash and dehydrate.

 

solution

time

number of changes

1X PBS

 

5 minutes

two

30% ethanol

 

30 seconds

one

60% ethanol

 

30 seconds

one

80% ethanol

 

30 seconds

one

90% ethanol

 

30 seconds

one

95% ethanol

 

30 seconds

one

100% ethanol

 

30 seconds

two

 

 

Store slides in an airtight container with a small amount of 100% ethanol in the bottom for up to several hours at 4°C.

 


B. Hybridization.

 

Organize the slides to be probed.  Slides will be sandwiched together as pairs.  Probe is applied to each individual pair.  Decide which pairs will be probed with sense strand probes (controls) and which will be probed with antisense strand probes.

 

1. Make hybridization solution (enough for 5 slide pairs):

 

100 microliters 10X in situ salts

400 microliters deionized formamide

200 microliters 50% dextran sulfate

20 microliters 50 X Denhardt’s

10 microliters 100 mg/ml tRNA

70 microliters DEPC-treated water

 

total volume: 800 microliters

 

The hybridization solution is very viscous from the dextran sulfate.  It can be warmed before using and/or you can make more than you need to make up for losses in dispensing.

 

Air dry the slides on a clean paper towel.  They must be completely dry. 

 

2. For each pair of slides, the desired amount of probe (see section on probe synthesis for suggested amount) should be added to 50% formamide so that the volume is 40 microliters.  Heat this solution to 80°C for 2 minutes.  Ice, spin down and keep on ice.  Add 160 microliters of hybridization solution to the 40 microliters of probe solution.  Mix without generating air bubbles. 

 

3.  Apply probe/hybridization solution mixture to slides.  200 microliters of the probe/hyb solution needs to be added to each slide pair.  One technique is to apply 100 microliters to each slide, spreading it out over the entire slide with the side of a pipette tip so that all of the tissue is exposed to probe.  Then slowly sandwich the slides together, avoiding air bubbles.  A second technique is to put all of the probe in the middle of one slide and slowly massage the other slide on top until the two slides are together.

 

Elevate the slide sandwiches  above  wet paper towels in an airtight plastic container.  Plastic serological pipettes can be used to raise the slides above the paper towels.  Place the container at 50 to 55°C overnight.

 

DAY TWO

 

A.  Wash slides

 

Warm 0.2X SSC to 55°C and NTE to 37°C.

 

Dip pairs of slides into prewarmed 0.2X SSC to separate and rinse them before placing in slide rack.  Carry out all washes with gentle agitation.

 

solution

time

temp

number of changes

0.2X SSC

 

60 minutes

55°C

two

NTE

 

5 minutes

37°C

two

RNAse (20 micrograms/ml in NTE)

30 minutes

37°

one

NTE

 

5 minutes

37°C

two

0.2X SSC

 

60 minutes

55°

one

1 X PBS

 

5 minutes

room temperature

one

 

 

B. Block and apply antibody

 

1.  Place slides face up on bottom of plastic container.  Wash 45 minutes with 1% Boehringer block (cat. #1096176) (made fresh following manufacturers directions) in 100 mM Tris, pH 7.5, 150 mM NaCl.  Use just enough of the solution to cover the slides and place on a rocking platform at room temperature.

 

2.  Replace block solution with 1% BSA in 100 mM Tris (pH7.5), 150 mM NaCl, 0.3% Triton X-100 for 45 minutes.

 

3.  Dilute the anti-digoxigenin antibody (Boehringer, cat#1093274) 1 to 1250 in the BSA/Tris/Triton solution from step 2.  Make a puddle of antibody solution in a plastic weigh boat.  Make slide “sandwiches” (two slides, tissue sides together).  Dip the long edge of the sandwich in the antibody solution and allow capillary action to pull the solution up into the gap between the slides.  Drain the solution onto a Kimwipe and repeat, avoiding air bubbles.

 

Place a layer of wet paper towels in an airtight plastic container.  Elevate the slides above the towels (for instance on a few disposable serological pipettes) and allow to sit at room temperature for 2 hours.

 

C.  Wash slides

 

1.  Drain the slides on Kimwipes and separate.  Place the slides face up in a single layer on the bottom of a plastic container.  Wash 4 times at room temperature, 15 minutes each time, with the BSA/Tris/NaCl/Triton solution.

 

2.  Wash once for ten minutes with 100mM Tris (pH 9.5), 100 mM NaCl, 50 mM MgCl2.  Then dip each slide in fresh Tris 9.5/NaCl/MgCl2 solution to ensure that all of the detergent is washed off.

 

D.  Apply substrate

 

Pour 10 mls of the NBT/BCIP premix (Western Blue from Promega, cat #S3841) into a plastic weigh boat.  Sandwich slides together, place edge of sandwich in solution and allow capillary action to draw the solution up between the slides.  Drain on a Kimwipe and repeat.  Place the slides in an airtight plastic container, elevated above wet paper towels.  Place the container in total darkness for one to three days.

 


DAY 3, 4 OR 5

 

Take down and mount slides

 

1.  You should peek at the slides periodically to monitor the color reaction.  When sufficient signal has developed, drain the solution onto a Kimwipe.  Lower the slides into a bath of TE to separate them and to stop the reaction.

 

2.  Dehydrate the slides - in this ethanol series it is important to keep the time in ethanol to a minimum (less than five seconds per solution) since the color product is soluble in ethanol.

 

solution

number of changes

30% ethanol

 

one

50% ethanol

 

one

70% ethanol

 

one

85% ethanol

 

one

95% ethanol

 

one

100% ethanol

 

two

100% Histoclear

 

two

 

3.  Drain and mount the slides in Cytoseal 60 (Stephens Scientific).

 

 


Recommended Stock Solutions for in situ hybridization

 

Solution

 

Composition

Remarks

 

10XPBS, pH 7

 

1.3 M NaCl

70 mM Na2HPO4

30 mM NaH2PO4