IN SITU PROTOCOL 1 OF 10
Making RNA Probes
Step 1: Digest Plasmid
Plasmid ____ (5ug/conc. of gene)
10X Buffer 15 ul
Enzyme (Kpn1) 2 ul
dH2O (no DEPC)Fill up to 150 ul
- Incubate at 37˚C for 1.5 hrs in water bath
- Remove and clean rxn using mini-Elute Kit (purple columns by Quaigen works best)
- Add 5 times volume of PBI Buffer to rxn mixture 750 ul
- Transfer to purple column (max volume at 700 ul)
- Centrifuge at 12 rpm for 1 min; repeat steps b-c until all volume is transferred
- Clean column with 750 ul of PE Buffer (make sure box is marked for addition of ethanol)
- Centrifuge and discard flow through
- Centrifuge for an additional minute and put column in new RNase free micro-centrifuge tube
- Elute with 10 ul of EB Buffer
- Run 1 ul on 1% TAE gel to visualize digest; make sure to also run a non-digested sample for comparison
Step 2: Transcription of probe
Plasmid2 ul (use 2 ul of the eluted 10 ul from previous step should be 1 ug)
10X Buffer2 ul
Enzyme mix2 ul
DIG label2 ul
DEPC H2O12 ul (To fill up to 20 ul)
- Incubate at 37˚C for 1.5 hrs in water bath
- Remove and clean rxn using mini-Elute kit
- Add 5X volume of PBI to rxn mixture 100 ul
- Transfer to purple column (max volume 700 ul)
- Centrifuge @ 12 rpm for 1 min
- Clean column with 750 ul of PE Buffer (make sure box is marked for addition of ethanol)
- Centrifuge and discard flow-through
- Centrifuge for an additional minute and put column in new RNase micro-centrifuge tube
- Elute RNA in 10 ul of DEPC H2O
- Add 41 ul DEPC H2O to a total volume of 50 ul
- Aliquot 1 ul into an 0.5 ml RNase free micro-centrifuge tube for gel running and another for Dot Blot
- Run 1 ul on a gel (1.5% TAE)usually run at 60 V for 2 hrs for good separation of ladder (RNA ladder = millennium marker)
- Store in -80˚C freezer until use
Revised Nguyen 10-4-06
IN SITU PROTOCOL 1 OF 10
Dot Blot for Concentration of Probe
Purpose: A dot blot is done on probe after it has been transcribed in order to calculate the quantity you have.
Safety: RNA-free wear gloves and lab coat at all times. ONLY pour ~10 ml of each soln in RNase treat box at a time so soln won’t overflow
Method: All steps take place on shaker and remember to thaw out solns prior to wash!
- Make serial dilutions (use 5 -1.5 ml micro-centrifuge tubes): Take correct ml from probe and follow arrows to dilute
1ul 2ul 2ul 5ul5ul
Tube #1 Tube #2 Tube #3 Tube #4 Tube #5
PROBE4ulRNA Buffer 2ul RNA Buffer 8ul RNA Buffer 5ul RNA Buffer 5ul RNA Buffer
Dilution: 5X 10X 50X 100X 200X
- Clean box with RNase ZAP and set up grid on nylon paper with pencil as example below: Add 1 ul of each dilution to appropriate grid position
5X / 10X / 50X / 100X / 200X
Control / • / • / • / • / •
Sample #1 / • / • / • / • / •
Sample #2 / • / • / • / • / •
So on… / • / • / • / • / •
- Bind RNA to filter using the spectrolinker press “optimal crosslink” and then “start” (don’t mess with time b/c time is already set)
- Work filter with 2X SSC for 10 mins
- Wash twice with PBT for 10 mins
- Preincubate filter with PI buffer for 1 hr
- Wash filter twice with PBT for 10 mins
- Incubate filter DIG AP (1/5000 dilution) in PI buffer for 30 mins
- For 10 ml DIG, add 200 ul of 1:100 DIG into 9800 ul PI
- Wash twice with PBT for 10 mins
- Dissolve 1 NBT tablet into 10 ml SDW (remember to use a new 15 ml tube each time and to cover with foil light sensitive); vortex to completely dissolve NBT tablet
- Incubate filter for 10 mins with NBT/SDW soln cover RNase treated box with foil
- Wash twice with PBT for 10 mins
- Stop rxn with 4% PFA
- Wash with 4% PFA for 5 min, take out with tweezer, dry nylon paper on paper towel
- Store nylon paper with sample to dry @ RT
Revised Nguyen 10-4-06
IN SITU PROTOCOL 1 of 10
IN SITU HYBRIDIZATION ON WHOLE MOUNTEMBRYOS
-All glassware must be baked overnight at 180˚ C
-Orange caps/plastic rings should be treated with RNase away, rinsed with distilled water and autoclaved.
-Gloves MUST be worn at all times.
Solutions
- 0.1% (v/v) DEPC-treated water store @ RT:
- Fill bottle up to 1L with milli-Q water. Add 1 ml DEPC (stored in 4˚C fridge). Add a stir-bar. Let stir overnight. Autoclave next day. Do not remove stir-bar. DEPC gets rid of RNase. Autoclaving gets rid of DEPC (or) else DEPC will destroy the enzymes used in the experiment.
- 4% Paraformaldehye (4% PFA) stored @ 4˚C or -20˚C:
- Measure 4 g Paraformaldehye (located in fridge). Add 10 ml of 10X PBS (in situ). Fill up to 100 ml with DEPC-treated water. Put in water bath at 65˚C. Add several drops of 10M NaOH until most PFA dissolve.
- 10X PBS (Phosphate Buffered Saline) stored @ RT:
- Mix 75.97g NaCL, 12.46g Na2HPO4· 2H2O (Dibasic), 4.14g NaH2PO4· H2O (monobasic, monohydrate). Dissolve in 800 ml DEPC-treated water. Adjust the pH to 7.0 with 1M NaOH and 1M HCl. Do not put the pH probe into the bottle (contamination!). Pour out some solution in a beaker. Check its pH. If more or less, adjust with HCl or NaOH by adding a few drops into the bottle. Pour some solution into the beaker. Check pH and so on….until pH is close to 7.0. Sterilize by autoclaving.
- 1X PBS stored @ RT:
- 100 ml 10X PBS diluted with approx. 900 ml DEPC-treated water up to 1L.
- PBT or PBST stored @ RT:
- To 1L of DEPC-treated 1X PBS, add 1 ml of 20% Tween.
- 20% Tween-20 stored @ RT:
- To make 100 ml volume, add 20 ml Tween-20 and fill up to 100 ml with DEPC-treated water.
- To make 10 ml add 2 ml Tween-20 and fill up to 10 ml with DEPC-treated water.
- 20X SSC (for hybridization and washing) stored @ RT:
- To make 1 L weigh 263.6 g of SSC Buffer powder (located in molecular biology cabinet) and fill up to 1 L with DEPC-treated water.
- Hybridization Buffer w/o tRNA stored @ -20˚C: (no probe use here)
- In a 50 ml tube, mix the following reagents: 32.5 ml formamide (this give 65% formamide final concentration), 12.5 ml 20X SSC/DEPC, 25 ul Heparin (100mg/ml), 50 ul 20% Tween, adjust pH to 6.0 with 0.5M Citric Acid (~920 ul) and fill up to 50 ml with DEPC-treated water.
- Hybridization buffer with tRNA (Hyb w/ tRNA) stored @ -20˚C:w/ probe added fresh
- With 50 ml of the hybridization buffer, add 500 ul of the yeast tRNA solution (stored @ -20˚C).
- Have 1% stock of tRNA, therefore, dilute 100X
- Ex) to make 3 ml, add 30 ul of 1% stock tRNA
- Heparin stored @ -20˚C:
- Located in Dr. Scemama’s cabinet in small bottle above microwave.
- Make a stock solution of 100mg/ml in DEPC-treated water. Store in aliquots at - 20˚C.
- AP Substrate Solution (NBT/BCIP tablets): Prepare fresh!
- Add 1 tablet to 10 ml of DEPC-treated water. Dissolve well by vortexing and cover with aluminum foil; or half a tablet with 5 ml of DEPC- treated water
- PI buffer (Pre-Incubation) stored @ -20˚C:
- For 50 ml: add 1.0 ml sheep serum (stored in 1 ml aliquots at - 20˚C), 100 mg BSA (Bovin Serum Albumin fraction V_@ 4˚C), fill up to 50 ml with PBT solution. Stored in 10 ml aliquots at - 20˚C!
- Alkaline Phosphate (AP) buffer – DIG AP buffer – for DIG label: Prepare fresh!
- Also known as Detective Buffer (10X dilute to 1X w/ SDW)
- In a 50 ml tube, mix 2.5 ml of 2M Tris base (pH 9.5), 2.5 ml of 1M MgCl2 (or MgCl2 hexahydrate), 1 ml of 5M NaCl, and 250 ul of 20% Tween. Adjust to 50 ml with sterile dH2O.
- 0.2X SSC stored @ RT:
- To make 50 ml final volume, add 500ul of 20X SSC and fill up to 50 ml with DEPC-treated water.
- 75% MetOH/PBT stored @ RT:
- For 50 ml, add 12.5 ml PBTto 37.5 ml MetOH
- 50% MetOH/PBT stored @ RT:
- For 50 ml, add25ml PBT to 25 ml MetOH
- 25% MetOH/PBT stored @ RT:
- For 50 ml, add 37.5 ml PBT to 12.5 ml MetOH
- Proteinase-K:
- Stored at - 20˚C. Stock is 20mg/ml which is 2000X concentrated. Dilute 5 ul of 20 mg/ml stock into 10 ml of PBT.
- Solution A
- 75% hybridization mix + 25% 2X SSC at 70˚C
- Solution B
- 50% hybridization mix + 50% 2X SSC at 70˚C
- Solution C
- 25% hybridization mix + 75% 2X SSC at 70˚C
- Anti-DIG antibody (pre-absorbed in PI buffer):
- 2 ul anti-DIG antibody + 198 ul PI Buffer = 200 ul
- 20 ul + 980 ul PI buffer = 1ml
- To make 10 ml, add 200 ul + 9800 ul (or 9.8ml) PI buffer = 10 ml
- This [10 ml] is PI – preabsorber anti-DIG antibody.
Revised Nguyen 10-4-06
IN SITU PROTOCOL 1 of 10
Prior to in situ:
- Fix embryos in freshly made PFA or “thawed” PFA 24 hrs after collecting embryos at RT in glass vials until ready to be wash with MetOH or next step.
- Transfer embryos accordingly to each solns below
- 1X 10 mins30%Methanol/DEPC
- 1X 10 mins50%Methanol/DEPC
- 1X 10 mins70%Methanol/DEPC
- 1X 10 mins100% Methanol
- 100% Methanol (embryos can be store here in -20˚C for further use)
IN SITU:
Day 1:
- Transfer fixed embryos from glass vials into RNase free micro-centrifuge tubes (in RNase free cabinet); turn on water bath and set it to 70˚C.
- Wash embryos at room temperature using 1ml on shaker:
- 1X 5 mins75%methanol/PBT
- 1X 5 mins 50%methanol/PBT
- 1X 5 mins 25%methanol/PBT
- 3X 5 mins each100%PBT
- Thaw out 4% PFA in water bath; take out when thawed.
- Digest with Proteinase-K according to the stage of development at room temp.
12 somites to 24h10 minutes
30-36hs15 minutes
48+20minutes - Add 0.5ul of 20mg/ml of stock proteinase-K into 1 ml 1X PBT (want final concentration to be 10ug/ul)
- REMEMBER: add 1ml 1X PBT into vials first before adding 0.5 ul of 20mg/ml of stock proteinase-K
- Aspirate (take out) proteinase-K immediately and refix with 4% PFA for 20 minutes at room temperature.
- Prewarm pre-hybridization and hybridization+tRNA at 70˚C in water bath.
- Rinse 5X in 1X PBT for five minutes each at room temperature.
- Rinse in pre-hybirdization one time for five minutes at 70˚C in water bath.
- Aspirate and transfer new pre-hybridization to micro-centrifuge tubes and incubate in water bath for three hours at 70˚C.
- Twenty minutes prior to finishing 3 hrs incubation, prepared probe in hybridization+tRNA and incubate (heat shock) at 80˚C for ten minutes
- Aspirate pre-hybridization solution and replace with probe+hybrdization+tRNA. Incubate at 70˚C in water bath for at least 16 hrs.
Day 2:
- Turn on Hybridization oven to 70˚C and do the following washes in Hyb. oven
- 10min 75% hyb mix+25% 2X SSC
- 10 min 50% hyb mix+50% 2X SSC
- 10 min 25% hyb mix+75% 2X SSC
- 10 min 100% 2X SSC
- Wash 2X for 15 minutes each with 0.2X SSC at 70˚C in hybridization oven (dilute 2X to needed soln w/ DEPC-treated water)
- Thaw out PI Buffer if needed or make PI Buffer
- Wash 2X for 5 minutes each with 50% 0.2X SSC+50% PBT at room temp
- Wash 2X for 5 minutes each with 100% PBT at room temp
- Incubate embryos in Pre-Incubation (PI) buffer for 5 min at room temp. (PI buffer= for 50 ml 49ml of PBT add 1ml sheep serum and 100mg Bovine S Albumin in fridge stored at -20˚C)
- Aspirate and replace with new PI buffer and incubate for 1 hour at room temp.
- Incubate with a 1:5000 final dilution in PI PRE-ABSORBED anti-DIG antibody at 4˚C overnight on the rocker. (Dilute stock of antibody (1:100) for 1.0ml, add 20ul of anti-body into 980ul PI buffer)
- Remember: Add PI buffer first before adding antibody.
Day 3:
- Wash 8X for 15 minutes each wash with PBT @ RT
- Wash 3X for 5 minutes DIG AP Buffer (ALWAYS made fresh) at room temperature.Use “DIG soln” box. Stock is 10X dilute to 1X DIG AP Buffer
- To make 40 ml 4 ml 10X DIG + 36 ml SDW
- After the third wash with DIG AP buffer, make AP substrate (NBT/BCIP tablet) solution at room temp and cover it in foil. Keep it in the dark on rotor.
- After last wash of DIG AP buffer, transfer samples to wells in micro-plate with big plastic pipette.
- Remove all DIG AP buffer making sure to not expose embryos to air for more then a few seconds
- HINT: do one well at a time.
- Add AP substrate (600 ul/well) to wells and cover microplate wells with aluminum foil. Set wells back onto shaker.
- HINT: Use new glass pipette during each new experiment
- Monitor color development every thirty minutes
- Stop reaction by washing with PBT quickly three times
- Fix embryos in 4% PFA overninght.
Revised Nguyen 10-4-06