Rapid analysis of the essential oil components of dried Zanthoxylum bungeanum Maxim by Fe2O3‐magnetic‐microsphere‐assisted microwave distillation and simultaneous headspace single‐drop microextraction followed by GC–MS

In this work, microwave distillation assisted by Fe₂O₃ magnetic microspheres (FMMS) and headspace single‐drop microextraction were combined, and developed for determination of essential oil compounds in dried Zanthoxylum bungeanum Maxim (ZBM). The FMMS were used as microwave absorption solid medium for dry distillation of dried ZBM. Using the proposed method, isolation, extraction, and concentration of essential oil compounds can be carried out in a single step. The experimental parameters including extraction solvent, solvent volume, microwave power, irradiation time, and the amount of added FMMS, were studied. The optimal analytical conditions were: 2.0 μL decane as the extraction solvent, microwave power of 300 W, irradiation time of 2 min, and the addition of 0.1 g FMMS to ZBM. The method precision was from 4 to 10%. A total of 52 compounds were identified by the proposed method. The conventional steam distillation method was also used for the analysis of essential oil in dried ZBM and only 31 compounds were identified by steam distillation method. It was found that the proposed method is a simple, rapid, reliable, and solvent‐free technique for the determination of volatile compounds in Chinese herbs.     

Tuning the solid-state emission of the analogous GFP chromophore by varying alkyl chains in the imidazolinone ring

New analogues of green fluorescent protein (GFP) chromophore mGFP-Cn (n = 1, 3, 5, 11) with alkyl chains of different lengths in the imidazolinone rings were synthesized and their crystal structures were determined. These GFP-like chromophores are all emissive in the solid state. And the solid-state emission quantum yields of increase by extending the lengths of alkyl chains, owing to the fact that the intermolecular pi-pi interactions are significantly weakened based on their crystal structures.     

HPLC-DAD data coupled with second-order calibration method applied to food analysis: Simultaneous determination of six benzoylurea insecticides in various fruit samples by selecting time region of chromatogram

This work presents a novel application of second-order calibration based on self-weighted alternating trilinear decomposition(SWATLD)algorithm for analyzing the HPLC-DAD data.The proposed method makes it possible to simultaneously determine teflubenzuron,hexaflumuron,flufenoxuron,chlorfluazuron,diflubenzuron and benzoylurea in different fruit samples,i.e.pear,apple and banana,in the selected time region of chromatogram.The concentration,elution time and spectral information of these benzoylurea insecticides are selectively extracted from complex matrices even in the presence of unknown interferences.The root-mean-square error of prediction(RMSEP)and figures of merit,including sensitivity(SEN),selectivity(SEL)and limit of detection(LOD)are employed to access the performance of the method.The LODs obtained for these insecticides are within the range 0.017–0.26 ppm in pears,0.039–0.33 ppm in apples,0.041–0.44 ppm in bananas,respectively.Such a chemometrics-based protocol holds great potential to be extended as a promising alternative for more practical applications in food safety and quality monitoring.     

Characterization of cellulose-based electrospun nanofiber membrane and its adsorptive behaviours using Cu(II), Cd(II), Pb(II) as models

Science China Chemistry - Nanofiber membranes from the composite of cellulose acetate/polyvinylpyrrolidone were prepared using electrospinning technique. After treated with water and alcoholic KOH...     

Chemical Regulation of Carbon Quantum Dots from Synthesis to Photocatalytic Activity

Carbon quantum dots (CQDs) were synthesized by heating various carbon sources in HNO₃ solution at reflux, and the effects of HNO₃ concentration on the size of the CQDs were investigated. Furthermore, the oxygen‐containing surface groups of as‐prepared CQDs were selectively reduced by NaBH₄, leading to new surface states. The experimental results show that the sizes of CQDs can be tuned by HNO₃ concentration and then influence their photoluminescent behaviors; the photoluminescent properties are related to both the size and surface state of the CQDs, but the photocatalytic activities are determined by surface states alone. The different oxygen‐containing groups on the surface of the CQDs can induce different degrees of the band bending upward, which determine the separation and combination of the electron–hole pairs. The high upward band bending, which is induced by C?O and COOH groups, facilitates separation of the electron–hole pairs and then enhances high photocatalytic activity. In contrast, the low upward band bending induced by C? OH groups hardly prevents the electron–hole pairs from surface recombination and then exhibits strong photoluminescence. Therefore, both the photocatalytic activities and optical properties of CQDs can be tuned by their surface states.     

Study of the Phase Transformation of Single Particles of Ga2O3 by UV‐Raman Spectroscopy and High‐Resolution TEM

By taking advantage of UV‐Raman spectroscopy and high‐resolution TEM (HRTEM), combined with the focused ion beam (FIB) technique, the transformation from GaOOH into α‐Ga₂O₃ and then into β‐Ga₂O₃ was followed. We found that the stepwise transformations took place from the surface region before developing into the bulk of single particles without particle agglomeration and growth. During the transformation from GaOOH into α‐Ga₂O₃, the elimination of water vapor through the dehydroxylation of GaOOH resulted in the formation of micropores in the single particles, whilst maintaining their particle size. For the phase transformation from α‐Ga₂O₃ into β‐Ga₂O₃, the nucleation of β‐Ga₂O₃ was found to occur at the surface defects and this process could be retarded by occupying these defects with a small amount of La₂O₃. By finely controlling the process of the phase transformation, the β‐Ga₂O₃ domains gradually developed from the surface into the bulk of the single particles without particle agglomeration. Therefore, the surface structure of the α‐Ga₂O₃ single particles can be easily tuned and a particle with an α@β core–shell phase structure has been obtained.     

Two lanthanum(III) complexes containing η2‐pyrazolate and η2‐1,2,4‐triazolate ligands: intramolecular C—H...N/O interactions and coordination geometries

The lanthanum(III) complexes tris(3,5‐diphenylpyrazolato‐κ²N,N′)tris(tetrahydrofuran‐κO)lanthanum(III) tetrahydrofuran monosolvate, [La(C₁₅H₁₁N₂)₃(C₄H₈O)₃]·C₄H₈O, (I), and tris(3,5‐diphenyl‐1,2,4‐triazolato‐κ²N¹,N²)tris(tetrahydrofuran‐κO)lanthanum(III), [La(C₁₄H₁₀N₃)₃(C₄H₈O)₃], (II), both contain La^III atoms coordinated by three heterocyclic ligands and three tetrahydrofuran ligands, but their coordination geometries differ. Complex (I) has a mer‐distorted octahedral geometry, while complex (II) has a fac‐distorted configuration. The difference in the coordination geometries and the existence of asymmetric La—N bonding in the two complexes is associated with intramolecular C—H...N/O interactions between the ligands.     

Reversible high‐temperature phase transition of a manganese(II) formate framework with imidazolium cations

A new metal–formate framework, poly[1H‐imidazol‐3‐ium [tri‐μ₂‐formato‐manganese(II)]], {(C₃H₅N₂)[Mn(HCOO)₃]}_n, was synthesized and its structural phase transition was studied by thermal analysis and variable‐temperature X‐ray diffraction analysis. The transition temperature is around 435 K. The high‐temperature phase is tetragonal and the low‐temperature phase is monoclinic, with a β angle close to 90°. The relationship of the unit cells between the two phases can be described as: a_HT = 0.5a_LT + 0.5b_LT; b_HT = −0.5a_LT + 0.5b_LT; c_HT = 0.5c_LT. In the high‐temperature phase, both the framework and the guest 1H‐imidazol‐3‐ium (HIm) cations are disordered; the HIm cations are located about 2mm sites and were modelled as fourfold disordered. The Mn and a formate C atom are located on fourfold rotary inversion axes, while another formate C atom is on a mirror plane. The low‐temperature structure is ordered and consists of two crystallographically independent HIm cations and two crystallographically independent Mn²⁺ ions. The phase transition is attributable to the order–disorder transition of the HIm cations.