AMPK Methods and Protocols

(Rick Simeone) #1

  1. Variable-temperature shaking incubator with fittings for
    12 2 L conical flasks.

  2. Centrifuges and rotors, e.g., Beckman-Coulter J6 with
    JA-25.50 rotor and Beckman-Coulter J6-M1 with JS 4.2 rotor.

  3. Sonicator fitted with microtip.

  4. Syringe filters 0.45μm.

  5. CompetentE. coliBL21 Star (DE3).

  6. Stock solution of ampicillin (100 mg/mL).

  7. 14 Luria-Bertani broth (LB) agar plates (with ampicillin
    100 μg/mL).

  8. 250μL SOC media.

  9. 10 L of Luria-Bertani broth (LB).

  10. IPTG: 100 mM isopropylβ-D-galactosidase (IPTG) in water.

  11. Lysis buffer: 50 mM Tris–HCl pH 8.0, 300 mM NaCl, 1 mM
    Tris(2-carboxyethyl)phosphine (TCEP), 20 mM imidazole,
    1 mM MgCl 2 , 4 EDTA-free protease inhibitor tablets
    (Roche Products Ltd), and 12μL benzonase.
    200 mL of lysis buffer is needed for washing pellets from
    12 0.8 L growth flasks (seeNote 1). Each 0.8 L culture
    typically yields 4–5 g of bacterial pellet.

  12. Nickel A buffer: 50 mM Tris–HCl pH 8.0, 300 mM NaCl,
    0.5 mM TCEP, and 20 mM imidazole.

  13. Nickel B buffer: 50 mM Tris–HCl pH 8.0, 300 mM NaCl,
    0.5 mM TCEP, and 400 mM imidazole.

  14. Gel filtration buffer: 50 mM Tris–HCl pH 8.0, 300 mM NaCl,
    and 0.5 mM TCEP.


2.2 Crystallization
Reagents
and Equipment



  1. 24- and 48-well crystallization plates (Hampton Research).

  2. Crystallization solution: 13% (w/v) polyethylene glycol (PEG)
    3350, 0.1 M MgCl 2 , 1% (w/v) glucose, 0.15% (w/v) cocami-
    dopropyl betaine (CAPB) in 100 mM imidazole at pH 6.2.

  3. Crystallization solution: 12% (w/v) PEG 3350, 300 mM
    guanidine-HCl in 100 mM piperazine-N,N^0 -bis(2-ethanesul-
    fonic acid) (PIPES) buffer at pH 7.2.

  4. 10 mM staurosporine in DMSO and 10 mM AMP in water.

  5. Ethylene glycol.

  6. Low-power (magnification 40) stereo microscope.

  7. Range of sizes (0.1–0.4 mm) 18 mm mounted cryoloop
    (Hampton Research Ltd).

  8. Liquid nitrogen for crystal freezing and storage.


AMPK Crystallisation 3
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