Buffers:
1x Lysis buffer (100 ml)
0.5% NP40 0.5
g
25
mM Tris pH 7.5 5
mls 0.5 M
100
mM NaCl 2
mls 5 M
50 mM NaF
0.21 g
add 1:250 mammalian protease
inhibitors just before use
Only for Y-Phosphorylation
experiments:
Add 1:100 Phosphatase Inhibitor
cocktail II
YP-IP Wash buffer (100 ml)
0.1
% NP40 0.1
g
25
mM Tris pH 7.5 5
mls 0.5 M
150
mM NaCl 3
mls 5 M
add 1:250 mammalian protease
inhibitors just before use
Only for Y-Phosphorylation
experiments:
add 1:100 Phosphatase Inhibitor
cocktail II
Protocol:
1. Swell some
ProteinA-sepharose (Pharmacia, fridge) in a large volume of millipore water in
a 15 ml conical and mix well to resuspend all the beads.
Wash the proteinA-sepharose
twice with ca. 10 bed-volumes of millipore water by pelleting the beads for 2
min at 1000 rpm in the Jouan. Then add 1 bed-volume of millipore or buffer to
one bed-volume of beads to get a
50% slurry.
2. Place dishes with cells on ice (metal plate on ice-bucket on a rocker) and wash three times with ice-cold PBS.
3. Add ice-cold
Lysis buffer to the dish. Use 0.4 ml for 6-well plate wells, 0.5 ml for 6 cm
dish,
1 ml for 10 cm dish and 2.5 ml for 15 cm dish. Keep rocking on ice for 15 min
(make sure buffer covers the whole surface).
4. Harvest the
cell lysate into 1.5 eppendorf tubes on ice. Keep samples on ice throughout the
procedure. Pellet any insoluble material for 3 min at top speed at 4¡C. Collect
the supernatant and discard the pellet.
5. Protein assay
the sample(s) (usually use 3 µl lysate from a 6 cm dish).
6. Distribute
equal amounts of lysate (usually 300-500mg protein) into
1.5 ml eppendorf tubes and add 5 µl of C-terminal anti-met (sc-10; Santa Cruz)
or 1ml of N-terminal anti-met
(DO-24; Upstate). Spin the stock for 1 min at top speed before adding to the
sample.
C-Terminal:
á
Add 30µl proteinA-sepharose (50% slurry) with a cut-off tip
(flick well to keep beads in suspension between pipetting).
á
Incubate on a wheel in the cold-room for 2 hours.
N-Terminal:
á
Incubate lysate+antibody on a wheel in the cold room
overnight.
á
Add 30ml
proteinA-sepharose (50% slurry).
á
Incubate on a wheel in the cold room for 2 hours.
7. Pellet beads
for 1 minute in eppendorf centrifuges at top speed Transfer unbound into fresh
tube and save on ice.
8. Wash beads 3x
with ice-cold YP-wash buffer. Pellet as above and remove all but 10-20 µl of
the wash to prevent losing beads.
9.
If the
IP is to be loaded on an SDS-PAGE, wash 1x with ice-cold 10 mM Tris pH 7.5 to
remove detergent, leave ~20 µl buffer on the beads and add 10 µl of 5x sample
buffer. (If the IP is to be used for other purposes use adequate buffer for the
final wash).
10. Store remaining beads in PBS + 1/1000 Thimerosal in the fridge
1 5ml of serum contains
between 40 and 80mg
of IgG. MW of IgG ~150kDa and the
valency of IgG is 2. Hence, 5ml of antiserum can bind 80-160mg of an antigen
of MW 150Kda.
2
25ml of ProteinA
sepharose is in vast excess for 5ml of Ab, but this is the minimum amount that is
easy to handle in a tube. If larger batches of protein are IPÕd the amount of
ProteinA sepharose to be used should be deduced from the binding capacity of
the beads (data sheet: 20mg of IgG/ml drained gel). The concentration of IgG in
serum is 8-16mg/ml. 5ml of serum hence contains 40-80mg of IgG and
2-4ml of ProteinA
sepharose (bed-volume) would be sufficient to IP all the antibody.