Avance 3 hd 600 nmr

Proton NMR spectra were recorded on an AVANCE III HD 600 NMR spectrometer (Ascend™ 600 magnet - Bruker Biospin Ltd.) operating at a frequency of 600.17 MHz for ¹H and equipped with a quadruple resonance CryoProbe (CPQCI 1H-31P/13 C/15 N) and a SampleJETTM autosampler. 1.5 mg of re-N-acetylated Pel was incubated with 20 µM of PelA_h in 1X PBS in D₂O for 60 h and transferred into a 3 mm NMR tube containing trimethylsilylpropanoic acid at a final concentration of 0.5 mM. Synthetic (α-1,4-GalNAc)₈-hexanoic acid, generously provided by Dr. Codée (Leiden University) served as a control. The ¹H spectra were acquired using the pulse sequence noesypr1d (Nuclear Overhauser Effect Spectroscopy 1D, Bruker Biospin Ltd) in order to achieve good suppression of the water signal. ¹H spectrum was acquired with 64 scans, a ¹H 90° pulse length of 7.8 μs, a mixing time of 10 ms, a spectral width of 12 kHz, and a recycle delay of 4 s for a total of 66 K data points. Anomer configuration was confirmed by 2D ¹H–¹H Correlation Spectroscopy (COSY) spectra at 25 °C with spectra acquired using 16 scans with a ¹H 90° pulse length of 8 μs, a spectral width of 3 kHz in both dimensions, a repetition delay of 1.8 s for a total of 2048 data points in F2 and 128 increments in F1. All spectra were processed using TOPSPIN software (version 3.5 pl 7, Bruker Biospin Ltd).

Malania oleifera Chun and S. K. Lee (simple name: Malania oleifera Chum) has been collected by the herbarium of Guangxi Institute of Botany, China, No.: IBK00373464. Malania oleifera Chum oil was extracted from fruit of Malania oleifera Chun harvested in Guangxi province of China. Plant species identified by Professor Lai Jiaye, botany expert (College of Forestry, Guangxi University). The consists of oils and fats 53.2%(w/w), in which the fats mainly contain 15-tetracosenic acid 46.7%, 9-octadecenoic acid 27.9%, and erucic acid 12.5%, other fatty acids 12.9%.
Standard cyclopentadecanone was purchased from Aldrich Co. (USA), purity: 98.0%. Standard cyclopentadecanolide was purchased from Askrich Chemical Company Inc. (Japan), purity: 98%. In order to In order to further verify the correctness of the synthetic product, the spectra (IR, GC-MS and NMR) of the synthetic product and the standard were compared. Hexane, Shanghai Adamas-β Co. (China), purity: 97.0%. Acetic acid, Shanghai Adamas-β Co. (China), purity: 99.5%.
IR spectra were recorded by a SHIMAZHU FT-IR8400S spectrometer (Japan). Mass spectra were determined by SHIMAZHU GC-MS/QP5050A (Japan). NMR spectra were recorded by AVANCE III HD 600 NMR (Bruker, Switizerland).