Structural damage and shear performance degradation of fiber–lime–soil under freeze–thaw cycling

The freeze–thaw cycling damages the soil structure, and the shear performance of soil are degraded. A series of tests on lime–soil(L–S) and fiber–lime–soil(F–L–S), including freeze–thaw test, the triaxial compression test, nuclear magnetic resonance (NMR) test and scanning electron microscope (SEM) test, were completed. The test results showed that fiber reinforcement changed the stress–strain behavior and failure pattern of soil. The cohesion and internal friction angle of soil gradually decreased with the increase of freeze–thaw cycles (F–T cycles). The pore radius and porosity of soil increased, while the micro pore volume decreased, and the small pore volume, medium pore volume and large pore volume increased, and the large pore volume had a little variation after 10 F–T cycles. The number of pores of F–L–S was less than L–S, demonstrating that the addition of fiber helped to reduce the pore volume. The interweaved fibers limited the development and the connection of cracks. By means of the spatial restraint effect of fiber on the soil and the friction action between fiber and soil, the shear performances and freeze–thaw durability of F–L–S better were than that of L–S.     

核磁共振波谱法测定臭氧化橄榄油中的活性成分含量

以橄榄油为原料,经臭氧氧化制备臭氧化橄榄油。利用核磁共振(NMR)采集碳谱数据,积分碳谱特征峰,计算橄榄油被氧化成分的相对含量。结果表明:臭氧化橄榄油与橄榄油碳谱有明显的区别,臭氧化橄榄油在δ103.1处出现新峰,对应δ130.1处的峰高减弱,这是由于橄榄油中的不饱和双键被氧化。采用该方法测得5个臭氧化油中活性成分含量分别为21.46%、21.03%、21.31%、18.71%和24.42%。采用核磁共振波谱法测定臭氧化橄榄油的活性成分含量具有操作简单,不需要预处理,结果可靠的优点。     

Proton Nuclear Magnetic Resonance-Based Method for the Quantification of Epoxidized Methyl Oleate

Epoxidized methyl esters (EMO) with their high oxirane ring reactivity, acts as a raw material in the synthesis of various industrial chemicals including polymers, stabilizers, plasticizers, glycols, polyols, carbonyl compounds, biolubricants etc. EMO has been generally quantified by the gas chromatography (GC) and high-performance liquid chromatography (HPLC) techniques. Taking into the account of the limitations of these techniques, two qHNMR-based equations have been proposed for the quantification of EMO in the mixture of EMO and methylesters (MO). The validity of the proposed method was determined using standard mixtures of MO and EMO having different molar concentrations. The developed equations have been applied on the samples of EMO prepared from oleic acid in two-step process viz., esterification followed by epoxidation. The qHNMR-based EMO quantification showed acceptable agreement with the results obtained from HPLC analysis.     

Characterisation of the Dynamic Interactions between Complex N-Glycans and Human CD22

CD22 (Siglec-2) is a B-cell surface inhibitory protein capable of selectively recognising sialylated glycans, thus dampening autoimmune responses against self-antigens. Here we have characterised the dynamic recognition of complex-type N-glycans by human CD22 by means of orthogonal approaches including NMR spectroscopy, computational methods and biophysical assays. We provide new molecular insights into the binding mode of sialoglycans in complex with h-CD22, highlighting the role of the sialic acid galactose moieties in the recognition process, elucidating the conformational behaviour of complex-type N-glycans bound to Siglec-2 and dissecting the formation of CD22 homo-oligomers on the B-cell surface. Our results could enable the development of additional therapeutics capable of modulating the activity of h-CD22 in autoimmune diseases and malignancies derived from B-cells.     

Mechanistic Studies on Trichoacorenol Synthase from Amycolatopsis benzoatilytica

Isotopic labeling experiments performed with a newly identified bacterial trichoacorenol synthase established a 1,5-hydride shift occurring in the cyclization mechanism. During EI-MS analysis, major fragments of the sesquiterpenoid were shown to arise via cryptic hydrogen movements. Therefore, the interpretation of earlier results regarding the cyclization mechanism obtained by feeding experiments in Trichoderma is revised.     

基于核磁共振代谢组学分析不同品种草莓的化学成分差异

目的采用基于核磁共振(nuclear magnetic resonance,NMR)的代谢组学方法对"丰香""久香""宁玉"和"甜查理"4个不同品种草莓进行指纹图谱比较和化学成分差异分析。方法采用主成分分析法综合评价4个不同品种草莓的整体分布状况;采用正交偏最小二乘判别分析法筛选并鉴别出引起不同草莓品种有所差异的潜在差异代谢物。结果研究发现,苹果酸在"丰香"草莓中含量最低,蔗糖含量则最高;蔗糖在"久香"草莓中的含量最低;丙氨酸、柠檬酸、天冬酰胺、D-葡萄糖和D-果糖在"宁玉"中含量最低;丙氨酸、苹果酸、柠檬酸、天冬氨酸和D-葡萄糖在"甜查理"中含量最高。结论基于NMR的代谢组学技术可以用于草莓品种的鉴别和化学成分的差异分析,并为草莓的品种溯源提供科学数据。     

Random poly(ε‐caprolactone‐L‐alanine) by direct melt copolymerization

A series of random polyesteramides (PEAs) with a range of molar composition from 90/10 to 50/50 were synthesized by direct melt polycondensation of ε‐caprolactone and l ‐alanine. Their structure was fully characterized by Fourier transform IR and NMR spectroscopy. The resulting copolymers are completely amorphous with the exception of PEA‐90/10 which possesses a semicrystalline structure. These PEAs present increasing glass transition temperatures at increasing l ‐alanine contents and exhibit fairly good thermal stability with 10% mass loss temperatures reaching 315 °C. © 2020 Society of Industrial Chemistry     

The Interfacial Interactions of Glycine and Short Glycine Peptides in Model Membrane Systems

The interactions of amino acids and peptides at model membrane interfaces have considerable implications for biological functions, with the ability to act as chemical messengers, hormones, neurotransmitters, and even as antibiotics and anticancer agents. In this study, glycine and the short glycine peptides diglycine, triglycine, and tetraglycine are studied with regards to their interactions at the model membrane interface of Aerosol-OT (AOT) reverse micelles via ¹H NMR spectroscopy, dynamic light scattering (DLS), and Langmuir trough measurements. It was found that with the exception of monomeric glycine, the peptides prefer to associate between the interface and bulk water pool of the reverse micelle. Monomeric glycine, however, resides with the N-terminus in the ordered interstitial water (stern layer) and the C-terminus located in the bulk water pool of the reverse micelle.     

Magnetic Resonance Signal Amplification by Reversible Exchange of Selective PyFALGEA Oligopeptide Ligands Towards Epidermal Growth Factor Receptors

The biorelevant PyFALGEA oligopeptide ligand, which is selective towards the epidermal growth factor receptor (EGFR), has been successfully employed as a substrate in magnetic resonance signal amplification by reversible exchange (SABRE) experiments. It is demonstrated that PyFALGEA and the iridium catalyst IMes form a PyFALGEA:IMes molecular complex. The interaction between PyFALGEA:IMes and H₂ results in a ternary SABRE complex. Selective 1D EXSY experiments reveal that this complex is labile, which is an essential condition for successful hyperpolarization by SABRE. Polarization transfer from parahydrogen to PyFALGEA is observed leading to significant enhancement of the ¹H NMR signals of PyFALGEA. Different iridium catalysts and peptides are inspected to discuss the influence of their molecular structures on the efficiency of hyperpolarization. It is observed that PyFALGEA oligopeptide hyperpolarization is more efficient when an iridium catalyst with a sterically less demanding NHC ligand system such as IMesBn is employed. Experiments with shorter analogues of PyFALGEA, that is, PyLGEA and PyEA, show that the bulky phenylalanine from the PyFALGEA oligopeptide causes steric hindrance in the SABRE complex, which hampers hyperpolarization with IMes. Finally, a single-scan ¹H NMR SABRE experiment of PyFALGEA with IMesBn revealed a unique pattern of NMR lines in the hydride region, which can be treated as a fingerprint of this important oligopeptide.     

Structure and crystallization behavior of complex mold flux glasses in the system CaO-Na2O-Li2O-CaF2-B2O3-SiO2: A multi-nuclear NMR spectroscopic study

The structure of mold flux glasses in the system CaO-(Na,Li)₂O-SiO₂-CaF₂ with unusually high modifier contents, stabilized by the addition of ∼4 mol% B₂O₃, is studied using ⁷Li, ²³Na, ¹⁹F, ¹¹B, and ²⁹Si magic-angle-spinning (MAS), and ⁷Li{¹⁹F} and ²³Na{¹⁹F} rotational echo double-resonance (REDOR) nuclear magnetic resonance (NMR) spectroscopy. When taken together, the spectroscopic results indicate that the structure of these glasses consists primarily of dimeric [Si₂O₇]⁻⁶ units that are linked to the (Ca,Na,Li)-O coordination polyhedra, and are interspersed with chains of corner-shared BO₃ units. The F atoms in the structure are exclusively bonded to Ca atoms, forming Ca(O,F)_n coordination polyhedra. This structural scenario is shown to be consistent with the crystallization of cuspidine (3CaO·2SiO₂·CaF₂) from the parent melts on slow supercooling. The progressive addition of Li to a Na-containing base composition results in a corresponding increase in the undercooling required for the nucleation of cuspidine in the melt, which is attributed to the frustrated local structure caused by the mixing of alkali ions.