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W Nerdal

Publications and source records attributed to W Nerdal.

16 recordsLinked to original sources

Structural restraints and heterogeneous orientation of the gramicidin A channel closed state in lipid bilayers.

Although there have been several decades of literature illustrating the opening and closing of the monovalent cation selective gramicidin A channel through single channel conductance, the closed conformation has remained poorly characterized. In sharp contrast, the open-state dimer is one of the highest resolution structures yet characterized in a lipid environment. To shift the open/closed equilibrium dramatically toward the closed state, a lower peptide/lipid molar ratio and, most importantly, long-chain lipids have been used. For the first time, structural evidence for a monomeric state has been observed for the native gramicidin A peptide. Solid-state NMR spectroscopy of single-site (15)N-labeled gramicidin in uniformly aligned bilayers in the L(alpha) phase have been observed. The results suggest a kinked structure with considerable orientational heterogeneity. The C-terminal domain is well structured, has a well-defined orientation in the bilayer, and appears to be in the bilayer interfacial region. On the other hand, the N-terminal domain, although appearing to be well structured and in the hydrophobic core of the bilayer, has a broad range of orientations relative to the bilayer normal. The structure is not just half of the open-state dimer, and neither is the structure restricted to the surface of the bilayer. Consequently, the monomeric or closed state appears to be a hybrid of these two models from the literature.

Anisotropy↗

Chlorpromazine interaction with glycerophospholipid liposomes studied by magic angle spinning solid state (13)C-NMR and differential scanning calorimetry.

Phosphatidylserine (PS) extracted from pig brain and synthetic dipalmitoylphosphatidylcholine (DPPC) and dimyristoylphosphatidylcholine (DMPC) were used to make DPPC/DMPC and DPPC/PS large unilamellar liposomes with a diameter of approximately 1 microm. Chlorpromazine-HCl (CPZ), an amphipathic cationic psychotropic drug of the phenothiazine group, is known to partition into lipid bilayer membranes of liposomes with partition coefficients depending on the acyl chain length and to alter the bilayer structure in a manner depending on the phospholipid headgroups. The effects of adding CPZ to these membranes were studied by differential scanning calorimetry and proton cross polarization solid state magic angle spinning (13)C-nuclear magnetic resonance spectroscopy (CP-MAS-(13)C-NMR). CP-MAS-(13)C-NMR spectra of the DPPC (60%)/DMPC (40%) and the DPPC (54%)/DMPC (36%)/CPZ (10%) liposomes, show that CPZ has low or no interaction with the phospholipids of this neutral and densely packed bilayer. Conversely, the DPPC (54%)/PS (36%)/CPZ (10%) bilayer at 25 degrees C demonstrates interaction of CPZ with the phospholipid headgroups (PS). This CPZ interaction causes about 30% of the acyl chains to enter the gauche conformation with low or no CPZ interdigitation among the acyl chains at this temperature (25 degrees C). The DPPC (54%)/PS (36%)/CPZ (10%) bilayer at a sample temperature of 37 degrees C (T(C)=31.2 degrees C), shows CPZ interdigitation among the phospholipids as deduced from the finding that approximately 30% of the phospholipid acyl chains carbon resonances shift low-field by 5-15 ppm.

Calorimetry, Differential Scanning↗

Physical properties of the transmembrane signal molecule, sn-1-stearoyl 2-arachidonoylglycerol. Acyl chain segregation and its biochemical implications.

sn-1,2-diacylglycerol (DAG), a key intermediate in lipid metabolism, activates protein kinase C and is a fusogen. Phosphoinositides, the main sources of DAG in cell signaling, contain mostly stearoyl and arachidonoyl in the sn-1 and -2 positions, respectively. The polymorphic behavior of sn-1-stearoyl-2-arachidonoylglycerol (SAG) was studied by differential scanning calorimetry, x-ray powder diffraction, and solid state magic angle spinning (MAS) (13)C NMR. Three alpha phases were found in the dry state. X-ray diffraction indicated that the acyl chains packed in a hexagonal array in the alpha phase, and the two sub-alpha phases packed with pseudo-hexagonal symmetry. In the narrow angle range strong diffractions of approximately 31 and approximately 62 A were present. High power proton-decoupled MAS (13)C NMR of isotropic SAG gave 16 distinct resonances of the 20 arachidonoyl carbons and 5 distinct resonances of the 18 stearoyl carbons. Upon cooling, all resonances of stearoyl weakened and vanished in the sub-alpha(2) phase, whereas arachidonoyl carbons from 8/9 to 20 gave distinct resonances in the frozen phases. Remarkably, the omega-carbon of the two acyl chains had different chemical shifts in alpha, sub-alpha(1), and sub-alpha(2) phases. Large differences in spin lattice relaxation of the stearoyl and arachidonoyl methene and methyl groups were demonstrated by contact time (cross-polarization) MAS (13)C NMR experiments in the solid phases alpha, sub-alpha(1), and sub-alpha(2). This shows that stearoyl and arachidonoyl in SAG have different environments in the solid states (alpha, sub-alpha(1), and sub-alpha(2) phases) and may segregate during cooling. The NMR and long spacing x-ray diffraction results suggest that SAG does not pack in a conventional double layer with the two acyls in a hairpin fashion. Our findings thus provide a physicochemical basis for DAG hexagonal phase domain separation within membrane bilayers.

Calorimetry, Differential Scanning↗

Interactions between Poly(Ethylene Oxide) and Sodium Dodecyl Sulfate as Studied by NMR, Conductivity, and Viscosity at 283.1-298.1 K

The aggregation of sodium dodecyl sulfate (SDS) in aqueous solution containing a constant amount of poly(ethylene oxide) (PEO) at 2000 ppm has been investigated by several experimental techniques at three temperatures, 298.1, 288.1, and 283.1 K. The techniques include conductivity, viscosity, NMR self-diffusion, NMR chemical shift, and NMR relaxation. The critical aggregation concentration of SDS on the polymer strand (cac) as well as the concentration where ordinary micelles start forming (c2) has been determined. There are some inconsistencies in the data due to different measuring techniques. However, techniques that basically monitor the SDS molecules, for instance conductivity and SDS-sensitive NMR techniques, provide cac values that are consistent. Above the cac the concentration of free SDS monomers will increase in parallel to the aggregation process. At c2 ordinary micelles will form, and in the concentration range of about 15-25 mmolal the SDS molecules will aggregate as normal micelles or in aggregates on the polymer, and these processes run in parallel. A crude calculation of the Gibbs' energy of the two aggregation processes suggests that the energetics of the two processes are of similar magnitude, and thus consistent with observation. Copyright 1998 Academic Press. Copyright 1998Academic Press

Journal Article↗

Sequence-dependent binding of metal ion to DNA oligomeres. A comparison of molecular electrostatic potentials with NMR data.

Experimentally observed sequence-selective binding of metal ion to DNA oligonucleotides have been compared with variations of electrostatic potential (EP) along the helix. Calculations of EP have been performed for three atomic models of the oligonucleotide duplex [d(CGCGAATTCGCG)2] using several variants of EP calculations, including a solution of non-linear Poisson-Boltzmann equation (NPBE). N7 atom of guanine adjacent to adenine base was identified as a region with the most negative electrostatic potential in the major groove. The EP value for the Me ion binding site surpasses the value for N7 of other guanines by 10-26% depending on particular duplex conformation. Qualitatively, the sequence dependent variations of EP near guanine N7 atoms are in agreement with the sequence-selective behavior of Mn(II) and Zn(II) ions as revealed by NMR experiments. But the difference in EP between the two most negative regions near guanine N7 atoms does not exceed 1.25 kT/e. Simple model suggests that metal ions are capable to form ion-hydrate complexes with G-Pu steps of DNA duplex. These complexes are formed via one Me...G and five Me...water coordination bonds with water molecules hydrogen bonded to two adjacent purine bases in the same chain. We suppose that such a stereospecific structural possibility is the main factor which control the sequence-selectivity in the metal ion binding. A combination of both mechanisms allows to explain sequence specific Mn(II) and Zn(II) binding to a set of oligonucleotides.

Computer Simulation↗

Sequence-selective interaction between mercury(II) ions and the DNA dodecamer [d(GCCGATATCGGC)]2 studied by 1H NMR spectroscopy.

The palindromic dodecamer [d(GCCGATATCGGC)]2 has been titrated by Hg(ClO4)2 in order to study sequence dependent HgII ion interactions. The titration pattern as monitored by 1D and 2D 1H NMR is consistent with a transition to a new conformer of the dodecamer induced by HgII ions. At intermediate stages of the titration, the proton signals from the new conformer coexist with those of the original one, indicating slow exchange between the two forms on the NMR timescale. The data clearly show that there is no major alteration in the secondary structure, e.g. B-->Z-form or duplex-->hairpin transition. The intra- and inter-residue sequential walk is completed except for a break between T6 and A7. At a concentration level r = [HgII]/[nucleobase] < 0.20 all four central imino signals are present. This definitely excludes thymine N3 as a possible mercuration site. In the imino region of the spectra HgII ions induce a large upfield shift of the thymine imino resonance T8-N3H, while the other thymine resonance T6-N3H is unperturbed. The guanine imino signal G4-N1H shows a large downfield ring current shift caused by major conformational changes in the duplex. The complete titration experiment indicates that mercury, initially, binds selectively to the A5'-T8 base pair. A tentative model is proposed where mercury is cross-linking the two strands via thymine T8-O4 and the deprotonated amino group of the complementary adenine base A5'.

Cross-Linking Reagents↗

Sequence-selective metal ion binding to DNA oligomers.

Sequence-selective interactions between DNA oligonucleotides and Pt(II) and Pd(II) complexes have been studied by 1D and 2D NMR spectroscopy. Titration of DNA oligomers with diamagnetic metal ion complexes induces chemical shifts of proton resonances close to the site of interaction. Conformational changes in the helical structure were monitored by measuring cross-peak intensities in 2D NOESY maps. Two duplex deoxynucleotides were studied, [d(CGCGCG)]2 and [d(CGCGAATTCGCG)]2, respectively. The hexamer was titrated in the duplex form with cis-[Pt(NH3)2Cl2]2+ (cis-DDP or cisplatin). The dodecamer was titrated with NO(3-)-salts of Pd(aq)2+, [Pd(en)(H2O)2]2+ and [Pd(dien)(H2O)]+, respectively. The reaction between cis-DDP and the hexamer at conditions where the duplex form is retained proceeded exceedingly slowly. In the initial phase of the titration the NOESY map indicates conformational changes induced by noncovalent adduct formation between the intact hexamer and cis-DDP. The more reactive Pd compounds show a tendency towards sequence-selective binding to the duplex dodecamer. The 'naked' Pd ion is very reactive and exhibits selectivity towards the thymine T8 imino proton and N7 on G4. At a Pd(II)/dodecamer ratio of 4:1 the metal ions induce helix-->coil transition. The mono- and bifunctional Pd complexes with 'bulky' ligands attack the dodecamer at the terminal GC base pairs, leaving the central Watson-Crick base pairs intact.

Base Sequence↗

Base dependence of B-DNA sugar conformation in solution and in the solid state.

Analysis of 1H-NOESY solution data for eight short DNA duplexes has revealed pronounced differences between the sugar conformations of purine and pyrimidine nucleotides. It was found that the H1'-H4' interproton distance is less than ca. 3.0 A in pyrimidine sugars, while in purine sugars it is more than ca. 3.0A. This difference has been analyzed by comparison with the sugar conformations of highly resolved B-DNA crystal structures and model sugar conformations. The conclusion can be drawn that the deoxyribose conformation is of the general C2'-endo type but pyrimidine sugars are characterized by smaller phase angles of pseudorotation P (90 degrees < P < 150 degrees), while purine sugars have larger P values that are greater than ca. 140 degrees (140 degrees < P < 180 degrees). There is no such clear base dependence of sugar conformation in highly resolved B-DNA crystal structures; however the similar trend can be seen as in the solution studies. Based on B-type DNA crystal structures, J-coupling constants have been calculated, and the applicability of experimental coupling measurements to the determination of sugar conformation is discussed.

Base Sequence↗

Evidence for double helical kappa-carrageenan in aqueous LiI-solution and model for iodide binding.

NMR experiments with a 21412 Redfield observation pulse were carried out on a kappa-carrageenan aqueous solution containing 0.5M LiI. A detected hydrogen-bonded proton resonance at approximately 17.6 ppm, is in accordance with an ordered carrageenan structure in the solution similar to the double, parallel-stranded helix with interstrand hydrogen-bonds found in the condensed state by R.P. Millane, R. Chandrasekaran, S. Arnott, and I.C.M. Dea (Carbohydr. Res. 198, 1 1988). Starting with the published iota-carrageenan coordinates obtained from the Brookhaven Databank, we modelled this kappa-carrageenan structure by the molecular modelling software INSIGHTH-II. The kappa-carrageenan double-helix has a wide interior that can accommodate iodide. Conversely, the iota-carrageenan double-helix has a narrow interior not suited for a large ion like iodide. We propose that the detected selective iodide binding sites in the ordered kappa-carrageenan structure (H. Grasdalen, and O. Smidsrød, Macromolecules 14, 1842 1981) could very well be in the interior of the double-helix.

Binding Sites↗

NMR studies of a plant flavonoid--DNA oligonucleotide complex.

A structural model of the solution complex between a flavonoid and a DNA dodecamer containing the E. coli wild-type lac promoter sequence (TATGTT) was obtained using simulated annealing for refinement. The distance constraints were derived from NOESY NMR spectra. The minor groove binding of this flavonoid displays possible hydrogen bonds to the DNA, and these can take part in complex formation. This work is the first description of how a molecule of this class of natural compounds may interact with DNA.

Base Sequence↗

Two-dimensional nuclear Overhauser enhancement NMR experiments on pelargonidin-3-glucopyranoside, an anthocyanin of low molecular mass.

Pelargonidin-3-glucoside has been isolated from the acidified methanolic extract of strawberries (Fragaria anannassa variety Corona) by successive application of an ion-exchange resin, droplet-counter chromatography and gel filtration. The pigment in acidified methanolic solution was studied by means of the two-dimensional nuclear Overhauser enhancement NMR technique, and the sugar unit was found to be attached to the 3-position on the aglycone. At +20 degrees C the pigment was found to be in the extreme narrowing limit where the NOESY cross-peaks are negative. However, at -20 degrees C this low-mass anthocyanin could be studied in the slow motion regime where the NOESY cross-peaks are positive. With a mixing time of 0.3 s, the glucose H1"-H4" proton pair was measured in the initial cross-relaxation rate and their cross-peak volume corresponded to the H1"-H4" distance found in a 4C1 chair conformation.

Anthocyanins↗

Cyanidin 3-[6-(p-coumaroyl)-2-(xylosyl)-glucoside]-5-glucoside and other anthocyanins from fruits of Sambucus canadensis.

From the fruits of Sambucus canadensis four anthocyanin glycosides have been isolated by successive application of an ion-exchange resin, droplet-counter chromatography and gel filtration. The structure of the novel, major (69.8%) pigment, cyanidin 3-O-[6-O-(E-p-coumaroyl-2-O-(beta-D-xylopyranosyl)-beta-D- glucopyranoside]-5-O-beta-D-glucopyranoside, was determined by means of chemical degradation, chromatography and spectroscopy, especially homo- and heteronuclear two-dimensional NMR techniques. The other anthocyanins were identified as cyanidin 3-sambubioside-5-glucoside (22.7%), cyanidin 3-sambubioside (2.3%) and cyanidin 3-glucoside (2.1%).

Anthocyanins↗

NMR distance measurements in DNA duplexes: sugars and bases have the same correlation times.

To evaluate whether the sugar moieties of short DNA duplexes exhibit local motion of sufficient amplitude to affect interproton distance measurements, we have carried out a series of time-dependent NOESY experiments at increasingly shorter mixing times on dodecamer DNA duplexes. By use of the cytosine H5-H6 vector as a known distance in the bases and the geminal 2'H-2''H vector as a known distance in the sugars, the corresponding apparent cross-relaxation rates were sampled at various mixing times. While the ratio of the inverse sixth power of these two fixed distances is in the range 6-7, when the system is sampled at 100 ms the apparent initial rate of growth of the 2'H-2''H NOESY crosspeak is only 1.9-2.0 times faster than that of the H5-H6 crosspeak--in agreement with the results of Clore and Gronenborn [Clore, G. M., & Gronenborn, A. M. (1984) FEBS Lett. 172, 219; (1984) FEBS Lett. 175, 117] and of Gronenborn and Clore [Gronenborn, A. M., & Clore, G. M. (1985) Prog. NMR Spectrosc. 17, 1]. This observation was interpreted to indicate the existence of internal mobility with a 3-fold shorter correlation time for the sugar moieties in DNA and led to the use of this shorter correlation time to estimate sugar-sugar proton distances and many sugar-base proton distances in subsequent DNA structure determination. We have examined 2'H-2"H cross-relaxation and H5-H6 cross-relaxation at 100, 90, 60, 30, and 15 ms in dodecamer DNA duplexes.(ABSTRACT TRUNCATED AT 250 WORDS)

Base Sequence↗

Solution structure of the EcoRI DNA sequence: refinement of NMR-derived distance geometry structures by NOESY spectrum back-calculations.

The solution structure of the self-complementary DNA duplex [d(CGCGAATTCGCG)]2, which contains the EcoRI restriction site sequence GAATTC at the center, has been studied by two-dimensional nuclear magnetic resonance spectroscopy. Time-dependent nuclear Overhauser effect spectra were used to obtain the initial cross-relaxation rates between 155 pairs of protons. These initial cross-relaxation rates were converted into interproton distances and entered into a distance (bounds) matrix. A distance geometry algorithm (DSPACE) was used to create embedded starting structures and to refine these structures until they showed good agreement with the distance matrix; symmetry constraints were included in the refinement procedure, making the two strands in the refined distance geometry structures virtually identical and significantly improving the agreement with the distance matrix. The NOESY spectrum for one of these distance geometry structures was then calculated from the explicit coordinates by numerically integrating all the z-magnetization transfer pathways among neighboring protons within a specified radius. Distances in this distance geometry structure that did not agree with the experimental NOESY time course were then adjusted accordingly. This process was iterated until a good agreement between calculated and experimental NOESY spectra was reached. The final structure, which generates good agreement with the experimental NOESY spectrum, displays kinks at the C3-G4 base step and at the A6-T7 base step that appear to be similar to those reported for the EcoRI restriction site DNA bound to its endonuclease. The solution structure is not the same as the crystal structure of this DNA duplex.

Base Sequence↗

Three-dimensional structure of the wild-type lac Pribnow promoter DNA in solution. Two-dimensional nuclear magnetic resonance studies and distance geometry calculations.

The solution structure of a 12 base-pair DNA duplex containing the wt-lac promoter Pribnow sequence TATGTT has been studied by two-dimensional nuclear magnetic resonance spectroscopy. Proton assignments for the 24 sugar and base residues were obtained from two-dimensional correlated nuclear magnetic resonance and two-dimensional nuclear Overhauser effect spectra in both 2H2O and H2O, and by two-dimensional relayed coherence transfer nuclear magnetic resonance spectroscopy experiments. Time-dependent, two-dimensional nuclear Overhauser effect spectra were used to determine the initial cross-relaxation rates between 212 pairs of assigned protons, leading to 212 interproton distances in the double helix (8 to 9 per nucleotide). These distance constraints, and known bond lengths and angles, were entered into a distance matrix. After smoothing the bounds of the distance matrix, 12 trial matrices within the bounds constraints were independently generated and embedded in three-dimensional space using a distance geometry algorithm, to generate 12 trial structures. These trial structures were then refined until they no longer violated the distance matrix. The resulting structures are very similar at the local base-pair and nearest-neighbor base-pair level, but exhibit increasing variation at more distant and global levels. At the nearest-neighbor level, the A to T step and the G to T step within the Pribnow hexamer, as well as the G to T step preceding the hexamer, all exhibit very low screw pitch, i.e. 5(+/- 6) degrees. Conversely, the T to G step in the center of the promoter has a large screw pitch (47(+/- 2) degrees) and the T to G step at the 3' end of the promoter has a very large screw pitch (60(+/- 3) degrees). The limitations of nuclear magnetic resonance spectroscopy distance determination of structure are discussed in terms of resolution and spectral overlap of two-dimensional nuclear Overhauser effect crosspeaks. In the present duplex, the inability to measure several 1'-2' and 1'-2" distances resulted in underdetermination of the precise local sugar conformation for seven of the 24 residues, although the spatial position of all sugars was well defined.

Base Sequence↗