Experiment OP - unpublished/hörstelCL/1

Article DOI N/A
Data DOI 10.57992/nmrxiv.p157.s1599
Internal ID unpublished/hörstelCL/1
Membrane composition (molar fraction)
TOCL 1’,3’-Bis[1,2-dioleoyl-sn-glycero-3-phospho]-glycerol 1
Solution composition
Compound Mass %
SOD 4.5
Temperature (K) 300.5
Total hydration 40 (mass %)
pH 8-10
Reagent sources
TOCL Avanti Polar Lipids
water Type I Milli-Q, degassed by argon bubbling
borax Sigma-Aldrich
boric_acid Sigma-Aldrich
Sample protocol TOCL/Na+ (30.0mg, 1.0 eq.) was dissolved with 10ml chloroform:methanol (2:1, v/v) in a 50ml pear shaped flask and the solvent was slowly evaporated under reduced pressure (250mbar, 40°C) to yield liposomes. A solution of Na2B4O17H20 (7.6mg, 1.0eq.) and BOH3 (4.9mg, 4.0eq.) in 5ml de- gassed water was prepared and added to the flask. Formed white flakes disapeared after rotating the flask at 800mbar for one minute. The Folch method was performed and 20ml chloroform:methanol (2:1, v/v) were added to the aqueous phase. An emulsion formed after shaking the mixture, a ho- mogeneous and clear solution formed after adding 3.3ml methanol. A phase separation occurred and the lower phase was dried under a constant stream of argon at 40°C over night. The predried sample was freeze-dried over night, 20.0µl degassed water was added and the Eppendorf was stored at 50°C for one day. Lost water was added and the sample was mixed thoroughly with a steel rod. After another day of equilibration the sample was again mixed before packing the insert. Hydration by 1H MAS NMR: 28 per phosphate, Na+ concentration guessed
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Name Value
ADDITIONAL_MOLECULES
Key Value
borax CAS: 1303-96-4
boric_acid CAS: 10043-35-3
PH_METHOD buffer
NMR
Key Value
INSTRUMENT Bruker Avance III HD 500 MHz, Triple Resonance CP-MAS Probe (4mm)
METHOD PDLF:R18_1^7
SIGN_MEASURED NONE
T_RF_HEATING measured
DETAILS 10.1016/j.jmr.2004.03.001, 5 kHz MAS

Order Parameters TOCL

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