cAMP Accumulation Assay

Reagent Preparation:

1. IBMX/DMEM ( 3-isobutyl-1-1-methylxanthine ( Sigma I 5879) ) ---- if need 100ml

Stock Solution: 50mM in 100% EtOH

Working Solution: 1mM in DMEM without serum

X/222.2

0.001= X=22.2 mg

100ml/1000

50mM x 10ˉ³ = 0.0222/222.2 Y=2.0ml

Y

Dissolve 22.2mg IBMX in 2.0ml 100% EtOH, then add to 98ml DMEM without serum.

2. 15 ml CRH-IBMX/ DMEM

Stocking CRH: 300 uM

Working CRH: 100 nM

12 ml x 100nM = Y x 300 x 10³ Y=4ul

Add 4ul CRH ( 300uM) to 12ml IBMX/DMEM

3. 40 ml Dox-IBMX/DMEM

Dox Stocking: 10ug/ul

Dox Working : 1.5ug/ml

40 ml x 1.5ug/ml = 60ug/ 10ug/ul=6.0ul

Add 6.0 ul of stocking Dox to 40 ml IBMX/DMEM

4. 12 ml CRH/Dox-IBMX/DMEM

Add 4ul CRH (300uM) and 1.8 ul Dox(10ug/ul) to 12 ml IBMX/DMEM

5. 0.1 N HCl --- 100ml

12N x Y = 0.1 x 100ml Y=0.83ml

Induction and Harvest Cells

· Aspirate media, add 1ml DMEM without serum

· Aspirate media, add another 1ml DMEM without serum

· Aspirate media, add 1ml Dox-IBMX/DMEM in Dox wells; add 1ml IBMX/DMEM in Non-Dox wells

· Incubate 1 hr at RT

· Aspirate media in CRH wells, add 1ml CRH/Dox-IBMX/DMEM in Dox/CRH wells; add 1ml CRH-IBMX/DMEM in CRH wells, add 1ml Dox-IBMX/DMEM in Dox wells and add 1ml IBMX/DMEM in the rest of wells ( without any labels). incubate 15 min at RT based on the following time points (T1):

T1(add CRH) T2(add 0.1N HCl) T3(Harvest) Samples

0 15 35 96-11, 96-21, 96-31, 96-41

1 16 36 96-12, 96-22, 96-32, 96-42

2 17 37 72-11, 72-21, 72-31, 72-41

3 18 38 72-12, 72-22, 72-32, 72-42

4 19 39 48-11, 48-21, 48-31, 48-41

5 20 40 48-12, 48-22, 48-32, 48-42

6 21 35 96-11, 96-21, 96-31, 96-41

7 22 36 96-12, 96-22, 96-32, 96-42

8 23 37 72-11, 72-21, 72-31, 72-41

9 24 38 72-12, 72-22, 72-32, 72-42

10 25 39 48-11, 48-21, 48-31, 48-41

11 26 40 48-12, 48-22, 48-32, 48-42

· After 15min incubation, aspirate media, add 500ul of 0.1N HCl based on T2,

· After 20min, pipette up and down cell media to lysis cells,

· Transfer cell lysate to 1.5 ml eppendof tube, keep on ice,

· Spin at 600g for 5min,

· Keep supernatant, do protein assay, then store at -20 for next day’s cAMP assay.

Protein Assay: Due to low protein concentration, we need use Bio-Rad method for protein assay (Range: 0-80ug/ml)

160 ul samples ( 1:5 or 1:8 dilution) or standard + 40 ul reagent ( 1:5 dilution) , check OD at 595nm

Stock BSA: 2000ug/ml

Final BSA Con(ug/ml) BSA to add (ul) 0.1N HCl to add (ul)

80 ( A ) 40 stock 960

40 ( B ) 500 ( A ) 500

20 ( C ) 500 ( B ) 500

10 ( D ) 500 ( C ) 500

5 ( E ) 500 ( D ) 500

2.5 ( F ) 500 ( E ) 500