Summary Pyrolysis-field ionization mass spectrometry (Py-FIMS) was used for the first time to directly characterize Chinese coals and their extracts. The summed mass spectra (about 30 magnetic scans) of four coal samples and the dimethylformamide extracts of two very different coals were registered between 50° and 750°C using linear heating in high vacuum (10–3 Pa) and approximately 6 min temperature rise time. Utilizing temperature-programmed pyrolysis and FI as soft ionization mode, the spectra displayed almost exclusively molecular ions of the evolved products. The thermograms, i.e. the intensities of the total ion current and selected ions were plotted versus the scan number, heating time and temperature. In general, two maxima in these thermograms were observed, which were different for the coals and reflected their carbon/hydrogen content. Comparing the mass spectra of the low temperature part (first maximum) with summed spectra of the extracts shows an interesting similarity. In contrast, the high temperature part (second maximum) indicates the products of thermo-degradation. The applied method is a fast and convenient tool for the characterization of evolved volatiles and thermal degradation products of coals and coal extracts.
Kennzeichnung von Kohlen mit direkter Pyrolyse und Feldionisations-Massenspektrometrie
[reaction: see text] A general reversed approach is described to synthesize S-palmitoylated and S-farnesylated peptides via S(N)2 displacement of bromide by reaction of a thiol group containing lipid as nucleophile with bromoalanine-containing peptides as electrophile. By employing this approach, lipidated peptides, including characteristic partial structures of human Ras peptides, were synthesized in good yields. This method gives access to farnesylated, palmitoylated, and doubly lipidated peptides. 相似文献
The development of a versatile platform that can separate oil/water mixture, remove dye from water, and purify wastewater is extremely desirable, yet still hard to realize. Herein, to address this challenge, a composite hydrogel was produced by freezing–thawing treatment using chitosan, polyvinyl alcohol, and carbon black as the raw materials. The obtained hydrogel displayed both slippery oil-repellency and water-affinity in air, underwater, when submerged in oil, and exploiting this special wettability, the hydrogel coated mesh can be used to separate oil/water mixtures efficiently. After 25 oil–water separation cycles, the hydrogel-coated filter still had a separation efficiency of over 98%. With its superhydrophilicity and active functional groups, the resulting hydrogel was able to absorb dye molecules dissolved in water effectively. Due to the photothermal effect of carbon black, the local temperature of the hydrogel was increasing quickly under sunlight illustration, which allowed it to be an advanced platform for daily wastewater purification through solar distillation.
Graphical abstract
A versatile hydrogel platform for oil–water separation, dye adsorption, and domestic wastewater purification was developed.
The solvation structure of Li+ plays a significant role in determining the physicochemical properties of electrolytes. However, to date, there is still no clear definition of the solvating power of different electrolyte solvents, and even the solvents that preferentially participate in the solvation structure remain controversial. In this study, we comprehensively discuss the solvating power and solvation process of Li+ ions using both experimental characterizations and theoretical calculations. Our findings reveal that the solvating power is dependent on the strength of the Li+-solvent (ion-dipole) interaction. Additionally, we uncover that the anions tend to enter the solvation sheath in most electrolyte systems through Li+-anion (ion-ion) interaction, which is weakened by the shielding effect of solvents. The competition between the Li+-solvent and Li+-anion interactions ultimately determines the final solvation structures. This insight into the fundamental understanding of the solvation structure of Li+ provides inspiration for the design of multifunctional mixed-solvent electrolytes for advanced batteries. 相似文献
A reliable method for determination of six α-dicarbonyl compounds in traditional Chinese medicines was first developed and validated by high-performance liquid chromatography-fluorescence detector with pre-column derivatization. α-Dicarbonyl compounds in traditional Chinese medicines were extracted and derivatized with 2,3-diaminaphthalene. The derivatization procedure of six α-dicarbonyl compounds was confirmed by high-resolution mass spectrometry. The limits of quantitation for six α-dicarbonyl compounds ranged from 3.70 × 10−3 to 2.21 × 10−2 μM. The established method showed good linearity (regression coefficient > 0.9990), precision (relative standard deviation < 3.37%), and high recovery (97.8%∼113.1%). The developed method was successfully applied to detect the six α-dicarbonyl compounds in traditional Chinese medicines. The result exhibited six α-dicarbonyl compounds was found in the 15 kinds of traditional Chinese medicines, which suggested us that the determination of α-dicarbonyl compounds should be paid more attention in the quality control of traditional Chinese medicines. 相似文献
A pre-column derivatization method for the sensitive determination of aldehydes using the tagging reagent 1,2-benzo-3,4-dihydrocarbazole-9-ethoxy-carbonylhydazine (BCEC) followed by high-performance liquid chromatography with fluorescence detection and enhance mass spectrometric identification has been developed. The chromophore of fluoren-9-methoxy-carbonylhydrazine (Fmoc-hydrazine) reagent was replaced by 1,2-benzo-3,4-dihydrocarbazole functional group, which resulted in a sensitive fluorescence derivatizing agent BCEC. BCEC can easily and quickly label aldehydes. The maximum excitation (333 nm) and emission (390 nm) wavelengths were essential no change for all the aldehyde derivatives. The fluorescence intensity was substantially affected by the solvents, being higher in organic than protic solvents. Derivatives are sufficiently stable to be efficiently analyzed by high-performance liquid chromatography. The derivatives showed an intense protonated molecular ion corresponding m/z [M + (CH2)n − 1]+ (M: molecular mass of BCEC, n: corresponding aldehyde carbon atom numbers) under positive-ion mode. The collision-induced dissociation of protonated molecular ion formed products at m/z = 245.7.0, m/z = 263.7 and m/z = 217.7, and corresponding the cleavage of CH2OCO, CH2OCO and NCH2CH2 bonds, respectively. Studies on derivatization demonstrated excellent derivative yields in the presence of trichloroacetic acid (TCA) catalyst. Maximal yields close to 100% were observed with a 10- to 15-fold molar reagent excess. Separation of the derivatized aldehydes has been optimized on ZORBAX Eclipse XDB-C8 column with aqueous acetonitrile in conjunction with a binary gradient elution. Excellent linear responses were observed at the concentration range of 0.08-16.65 μmol/L with coefficients of >0.9999. Estimated detection limits for the aldehydes, obtained by successive dilution of a derivatized standard solution containing 16.65 μmol/L of each aldehyde (at a signal-to-noise ratio = 3:1), are from 3.75 to 16.65 fmol. 相似文献