Experiment OP - unpublished/hörstelCL/2

Article DOI N/A
Data DOI 10.57992/nmrxiv.p157.s1600
Internal ID unpublished/hörstelCL/2
Membrane composition (molar fraction)
TOCL 1’,3’-Bis[1,2-dioleoyl-sn-glycero-3-phospho]-glycerol 1
Solution composition
Compound Mass %
CLA 2.7
SOD 4.9
TMA 8
Temperature (K) 300.5
Total hydration 42 (mass %)
pH 8-10
Reagent sources
TOCL Avanti Polar Lipids
water Type I Milli-Q, degassed by argon bubbling
TMACl Sigma-Aldrich
boricacid Sigma-Aldrich
Sample protocol TOCL/Na+(30.0mg,1.0 eq.) and TMACl(6.6mg,3.0eq.) were dissolved with2mlchloroform:methanol (2:1, v/v) in an eppendorf vial. A solution of TMA OHx5H2O (3.6mg, 1.0eq.) and BOH3 (1.2mg, 1.0eq.) in 100µl methanol was prepared and added to the Eppendorf vial. The Folch method was performed and 0.4ml degassed water was added to the mixture. After an immediate phase separa- tion, the upper phase was discarded, the solvent of the lower phase was evaporated at 40°C under a constant stream of argon and the predried sample was freeze-dried over night. 32.4µl 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 three days of equilibration the sample was again mixed before packing the insert. Hydration by 1H MAS NMR: 34 per phosphate, Na+ and B concentration estimated from ICP-OES, TMA+ concentration estimated from 1H MAS NMR
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Name Value
ADDITIONAL_MOLECULES
Key Value
boric_acid CAS: 10043-35-3, 0.5%
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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