How to Install Microsoft Office 2019 Video Tutorial Guide How to Install Adobe Premiere Pro CC 2019 Video Tutorial Guide How to Install Windows Repair Pro 2018 Video Tutorial Guide #Mestrenova Tutorial How To Install MestReNova#.#Mestrenova Tutorial Manual Software Also#.1D 13C spectra were processed using zero-filling from 64 to 128 k, line broadening 1 Hz, manual phase correction and five-degree polynomial baseline correction on the whole spectral window. For both HSQC and HMBC spectra, unless otherwise specified, relaxation delay D1 was set to 1.5 s.įor HSQC experiments, five sequences were used ( Supplementary Materials, Figure S1):ġD and 2D spectra were processed using Topspin software (Bruker Biospin, Billerica, MA, USA). For HSQC spectra, broadband decoupling during acquisition was obtained with the standard GARP scheme, and unless otherwise specified interpulse INEPT delay was optimized for a 145 Hz J value for the cyclosporin sample and 132 Hz for polymer samples.
13C spectral window was 12 or 4 ppm for cyclosporin and polymer sample, respectively, and 256 t 1 increments were used. Bs 2D HSQC and HMBC spectra were acquired using following parameters: 1H spectral window was 9.2 or 8.0 ppm for cyclosporin and polymer samples, respectively, resulting in acquisition time of 0.44 or 0.51 s, respectively (TD 4096).
Acquisition time was 1.05 s and relaxation delay D1 2.00 s. 1D 13C spectra were acquired using Bruker standard zgpg30 sequence (30° flip angle, bilevel 1H Waltz-16 decoupling). Polymer samples were prepared by dissolving about 35 mg of solid in ca. The cyclosporin sample was a sealed sample containing 50 mg of cyclosporin A in 0.5 mL of C 6D 6.
Herein is reported an evaluation of various bs-HSQC and bs-HMBC sequences, first from a methodological point of view (selectivity, dependence to INEPT interpulse delay or relaxation delay), using the cyclic peptide cyclosporin selected as a model compound, and then from an applicative approach, comparing tacticity determined from bs-HSQC and bs-HMBC experiments to the one obtained from 1D 13C on the carbonyl region.ġD and 2D NMR spectra were recorded on a 500 MHz Bruker Av III HD spectrometer (Billerica, MA, USA), fitted with a direct broadband 5 mm probehead (BBO) carefully tuned on both 1H and 13C channels. Band-selective (bs) HSQC, improving spectral resolution by restriction of the heteronuclear dimension without inducing spectral folding, has been recently used for polymer tacticity determination.
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