% IMPORTANT: The following is UTF-8 encoded. This means that in the presence
% of non-ASCII characters, it will not work with BibTeX 0.99 or older.
% Instead, you should use an up-to-date BibTeX implementation like “bibtex8” or
% “biber”.
@MISC{Gilsbach:276097,
author = {Gilsbach, Bernd and Ho, Franz Y. and Zhang, Xiaojuan and
Kortholt, Arjan and Gloeckner, Christian Johannes},
title = {{D}ataset: {S}upplemental data for '{I}ntramolecular
feedback regulation of the {LRRK}2 {R}oc {G} domain by a
{LRRK}2 kinase dependent mechanism' ({G}ilsbach et al.,
e{L}ife 2024, doi:10.7554/e{L}ife.91083), v3},
publisher = {Zenodo},
reportid = {DZNE-2025-00178},
year = {2024},
abstract = {Supportive data for the eLife version of record. (1) Data
used for the Michaelis Menten Kinetics. HPLC-based assay.
Steady-state kinetic measurements of LRRK2-mediated GTP
hydrolysis were performed as previously described (Ahmadian
et al., 1997). Briefly, 0.1 µM of full-length LRRK2 was
incubated with different amounts of GTP (0, 25, 75, 150,
250, 500, 1000, 2000, 3000 and 5000 µM) and production of
GDP was monitored by reversed phase C18 HPLC. To this end,
the samples (10 µl) were directly injected on a
reversed-phase C18 column (pre-column: Hypersil Gold, 3µm
particle size, 4.6x10mm; main column: Hypersil Gold, 5µm
particle size, 4.6x250mm, Thermo Scientific) using an
Ultimate 3000 HPLC system (Thermo Scientific, Waltham, MA,
USA) in HPLC-buffer containing 50 mM KH2PO4/K2HPO4 pH 6.0,
10 mM tetrabutylammonium bromide and $10-15\%$ acetonitrile.
Subsequently, samples were analyzed using the HPLC
integrator (Chromeleon 7.2, Thermo Scientific, Waltham, MA,
USA). Initial rates of GDP production were plotted against
the GTP concentration using GraFit5 (v.5.0.13, Erithacus
Software). The number of experiments is indicated in the
graph and data point is the average (±s.e.m.) of indicated
repetitions. The Michaelis-Menten equation was fitted to
determine KM (±s.e.) and kcat (±s.e.). Excel sheets used
for the calculation of means are provided. No values are
reported if the HPLC separation failed (e.g. unstable
baseline). Charcoal GTP hydrolysis assay. The [γ-32P]GTP
charcoal assay was performed as previously described (Bollag
and McCormick, 1995). Briefly, 0.1 µM full-length LRRK2 or
0.5 µM 6xHIS-MBP-RocCOR was incubated with different GTP
concentrations, ranging from 75 µM to 8 mM, in the presence
of [γ-32P] GTP in GTPase assay buffer (30 mM Tris pH 8, 150
mM NaCl, 10 mM MgCl2, $5\%$ (v/v) Glycerol and 3 mM DTT).
Samples were taken at different time-points and immediately
quenched with $5\%$ activated charcoal in 20 mM phosphoric
acid. All non-hydrolyzed GTP and proteins were stripped by
the activated charcoal and sedimented by centrifugation. The
radioactivity of the isolated inorganic phosphates was then
measured by scintillation counting. The initial rates of
γ-phosphate release and the Michaelis-Menten kinetics were
calculated as described above. (2) Profile plots (Raw data)
obtained for the Mass photometry analysis for T1343A vs WT
LRRK2. MP was performed as described in (Guaitoli et al.,
2023). Briefly, the dimer ratio of LRRK2 was determined on a
Refeyn Two MP instrument (Refeyn). Prior to the experiment,
a standard curve relating particle contrasts to molecular
weight was established using a Native molecular weight
standard (Invitrogen, 1:200 dilution in HEPES-based elution
buffer: 50 mM HEPES [pH 8.0], 150 mM NaCl supplemented with
200 µM desthiobiotin). Prior to mass photometry, the
proteins, either WT or T1343A LRRK2, were incubated with 0.5
mM ATP or buffer (control) for 30 min at 30 ℃. The LRRK2
protein was diluted to 2x of the final concentration (end
concentrations: 75 nM and 100 nM) in elution buffer. The
optical setup was focused in 10 μl elution buffer before
adding 10 µl of the adjusted protein sample. Depending on
the obtained count numbers, acquisition times were chosen
between 20 s to 1 min. The dimer ratio in each measurement
was normalize according to the equation. The measurement was
perfomed in triplicates. (3) AlphaFold3 model of
LRRK2-pT1343 either bound to GDP/Mg or GTP/Mg. Using
AlphaFold3 (Abramson et al., 2024), we modeled and compared
the GDP vs the GTP-state of phospho-T1343 LRRK2.
Interestingly, the AlphaFold3 model suggests, that the
phosphate group of the pT1343 residue is orientated inwards
thereby substituting the gamma phosphate of the GTP in the
GDP-bound state of LRRK2. This finding is in well agreement
with MD simulations published recently (Stormer et al.,
2023). (4) Western blot RAW files for the cell-based phospho
Rab asssay (RAW data for Figure 6 supplement 2/ Supplemental
Figure 4 in the preprint version, Gilsbach et al, 2024)
Cell-based LRRK2 activity assays were performed as
previously described (Singh et al., 2022). Briefly, HEK293T
cells were cultured in DMEM (supplemented with $10\%$ Fetal
Bovine Serum and $0.5\%$ Pen/Strep). For the assay, the
cells were seeded onto six-well plates and transfected at a
confluency of $50-70\%$ with SF-tagged LRRK2 variants using
PEI-based lipofection. After 48 hours cells were lysed in
lysis buffer [30 mM Tris-HCl (pH7.4), 150 mM NaCl, $1\%$
NonidentP-40 substitute, complete protease inhibitor
cocktail, PhosStop phosphatase inhibitors (Roche)]. Lysates
were cleared by centrifugation at 10,000 x g and adjusted to
a protein concentration of 1 µg/µl in 1x Laemmli Buffer.
Samples were subsequently subjected to SDS PAGE and Western
Blot analysis to determine LRRK2 pS935 and Rab10 T73
phosphorylation levels, as described below. Total LRRK2 and
Rab10 levels were determined as a reference for
normalization. For Western blot analysis, protein samples
were separated by SDS–PAGE using NuPAGE $10\%$ Bis-Tris
gels (Invitrogen) and transferred onto PVDF membranes
(Thermo Fisher). To allow simultaneous probing for LRRK2 on
the one hand and Rab10 on the other hand, membranes were cut
horizontally at the 140 kDa MW marker band. After blocking
non-specific binding sites with $5\%$ non-fat dry milk in
TBST (1 h, RT) (25 mM Tris, pH 7.4, 150 mM NaCl, $0.1\%$
Tween-20), membranes were incubated overnight at 4°C with
primary antibodies at dilutions specified below.
Phospho-specific antibodies were diluted in TBST/ $5\%$ BSA
(Roth GmbH). Non-phospho-specific antibodies were diluted in
TBST/ $5\%$ non-fat dry milk powder (BioRad). Phospho-Rab10
levels were determined by the site-specific rabbit
monoclonal antibody anti-pRAB10(pT73) (Abcam, ab230261) and
LRRK2 pS935 was determined by the site-specific rabbit
monoclonal antibody UDD2 (Abcam, ab133450), both at a
dilution of 1:2,000. Total LRRK2 levels were determined by
the in-house rat monoclonal antibody anti-pan-LRRK2 (clone
24D8; 1:10,000) (Carrion et al., 2017). Total Rab10 levels
were determined by the rabbit monoclonal antibody
anti-RAB10/ERP13424 (Abcam, ab181367) at a dilution of
1:5,000. For detection, goat anti-rat IgG or anti-rabbit IgG
HRP-coupled secondary antibodies (Jackson ImmunoResearch)
were used at a dilution of 1:15,000 in TBST/ $5\%$ non-fat
dry milk powder. Antibody–antigen complexes were
visualized using the ECL plus chemiluminescence detection
system (GE Healthcare) using the Stella imaging system
(Raytest) for detection and quantification. Figure 6 Source
Data 1: Images generated by the Stella system are shown
which were used for quantification. The annotation file
equals Figure6-figure supplement 2 (Gilsbach et al., eLife
2024, doi:10.7554/eLife.91083). The lines corresponding to
LRRK2 pS935, total LRRK2, Rab10 pT73 and total Rab10 were
used for the quantification shown in Figure 6.},
keywords = {structural modeling (Other) / LRRK2 (Other)},
cin = {AG Gloeckner},
cid = {I:(DE-2719)1210007},
pnm = {352 - Disease Mechanisms (POF4-352)},
pid = {G:(DE-HGF)POF4-352},
typ = {PUB:(DE-HGF)32},
doi = {10.5281/ZENODO.14055918},
url = {https://pub.dzne.de/record/276097},
}