Development and validation of an ultra high‐performance liquid chromatographic method for the determination of a diastereomeric impurity in (+)‐pinoresinol diglucoside chemical reference substance

(+)‐Pinoresinol 4,4′‐di‐O‐β‐D ‐glucopyranoside ((+)‐PDG) is one of the major lignans with various pharmacological activities which could be isolated from Duzhong and other plant species. In this study, a diastereomeric impurity, (?)‐pinoresinol 4,4′‐di‐O‐β‐D ‐glucopyranoside ((?)‐PDG), the main impurity was identified in (+)‐PDG chemical reference substance (CRS) and a reliable chromatographic method for rapid purity determination of (+)‐PDG CRS was firstly developed. The optimal chromatographic condition was found to be using ACN/1,4‐dioxane–water (2.5:6:91.5, v/v/v) as mobile phase on a Waters Acquity UPLC HSS T3 column (2.1 mm×100 mm, 1.8 μm) with column temperature of 37°C. The method was validated and applied to determine the chromatographic purity of five (+)‐PDG CRS samples. The content of (?)‐PDG in four commercial (+)‐PDG CRS was 8.47–20.30%, whereas no (?)‐PDG was detected in our in‐house prepared (+)‐PDG CRS in which purity was confirmed to be 99.80%. The above results confirmed that this method is fast and highly efficient for purity determination of the (+)‐PDG CRS.     

Thermo‐ and Acid‐Responsive Photochromic Spironaphthoxazine‐Containing Organogelators

A series of photochromic spironaphthoxazine derivatives has been designed, synthesized, and characterized by using ¹H NMR spectroscopy, FAB mass spectrometry, and elemental analysis. Their photophysical and photochromic behavior have been investigated. Two of the compounds (G¹²‐en‐SA‐SO and G¹⁶‐en‐SA‐SO) have been shown to be capable of forming stable thermoreversible organogels in organic solvents, tested by the “stable‐to‐inversion of a test tube” method. Addition of p‐toluenesulfonic acid was found to induce the formation of stable organogels at concentrations below that of the critical gelation concentration (c.g.c.), with a concomitant change in color from colorless to purple. Transmission electron microscopy and scanning electron microscopy of the xerogels showed typical fibrous structures in the micrometer scale. The activation parameters for the bleaching reaction of G⁸‐en‐SA‐SO in the solution state and G¹⁶‐en‐SA‐SO in the gel state have been determined in ethanol through kinetic studies at various temperatures. The results showed that the rate of the bleaching reaction in the gel state was much slower than that in the solution state.     

Data fusion in multivariate calibration transfer

We report the use of stacked partial least-squares regression and stacked dual-domain regression analysis with four commonly used techniques for calibration transfer to improve predictive performance from transferred multivariate calibration models. The predictive performance from three conventional calibration transfer methods, piecewise direct standardization (PDS), orthogonal signal correction (OSC) and model updating (MUP), requiring standards measured on both instruments, was significantly improved from data fusion either by stacking of wavelet scales or by stacking of spectral intervals, as demonstrated by transfer of calibrations developed on near-infrared spectra of synthetic gasoline. Stacking did not produce as significant an improvement for calibration transfer using a finite impulse response (FIR) filter, but application of SPLS regression to FIR-transferred spectra improves predictive performance of the transferred model.     

荧光法快速检测有机磷农药残留总量

在pH4.60的B-R缓冲溶液中,中性红(NR)与一定浓度的十二烷基苯磺酸钠(SDBS)发生荧光增强反应,在该体系中加入有机磷农药后,在激发波长560 nm,发射波长604 nm处体系的荧光强度明显降低,且降低程度与有机磷农药的加入量呈良好的线性关系,其线性范围和检出限分别为0.024~0.40 mg/L,0.014 mg/L。据此建立了测定有机磷农药残留总量的新方法。方法已用于面粉和土壤中有机磷农药残留总量的检测,回收率在92.0%~100.5%之间,RSD在1.1~1.9%之间。     

Charged particle coherent states in tomographic probability representation

The symplectic tomograms of coherent states of a charged particle moving in a constant uniform magnetic field are obtained in explicit form. The tomograms are shown to coincide with normal probability distributions of two random variables. The means and dispersions of the variables are found and expressed in terms of means and dispersions of the charged particle coordinates and momenta. The characteristic function of the tomographic probability distribution is found. The center of mass tomogram of the coherent state of charge in magnetic field is also found and the relation of the symplectic tomogram and the center of mass tomogram is established.     

Graphene-based passively Q-switched diode-side-pumped Nd:YAG solid laser

In this paper, a desirably simple, convenient and inexpensive saturable absorber mirror has been fabricated based on graphene, which has no wavelength selectivity. Moreover, there are no changes in the structure and characteristics of graphene. By inserting the graphene-PMMA SA mirror to the Nd: YAG laser, the shortest pulse width of 260 ns can be obtained with the single-pulse energy of about 8.32 μJ. The experimental results prove that our graphene-PMMA SA mirror is feasible and suitable for Q-switched lasers.     

Probability representation and state-extended uncertainty relations

The new inequality recently found by Trifonov and called the state-extended inequality is considered in the tomographic-probability representation of quantum mechanics. The Trifonov uncertainty relations are expressed in terms of optical tomograms and can be checked in experiments on homodyne detection of the photon states.     

Structural and magnetic properties of nanocrystalline bismuth manganite obtained by mechanochemical synthesis

We have studied the formation of BiMnO3 (BMO) nanocrystalline perovskite powder produced by high-energy milling of the constituent oxides. The crystal structure and the amount of crystalline and amorphous phases in the powder as a function of the milling time were determined with XRPD using Rietveld refinement. BMO perovskite formed directly from highly activated nano-sized constituent oxides after 240 min of milling and subsequently grew during prolonged milling. The morphology, structure, and chemical composition of the powder were investigated by SEM and TEM. A clear ferromagnetic transition was observed at T _C ~66 K for a sample milled for 240 min and increased with milling time. The magnetic hysteresis behavior is similar to that of a soft ferromagnet. The magnetic properties of the obtained BMO powders were found to change as a function of milling time in a manner consistent with variations in the nanocomposite microstructure.     

The important role of Mn in the room-temperature ferromagnetism of Mn-doped GaN films

Mn-doped GaN films (Ga_1−xMn_xN) were grown on sapphire (0 0 0 1) using Laser assisted Molecular Beam Epitaxy (LMBE). High-quality nanocrystalline Ga_1−xMn_xN films with different Mn concentration were then obtained by thermal annealing treatment for 30 min in the ammonia atmosphere. Mn ions were incorporated into the wurtzite structure of the host lattice by substituting the Ga sites with Mn³⁺ due to the thermal treatment. Mn³⁺, which is confirmed by XPS analysis, is believed to be the decisive factor in the origin of room-temperature ferromagnetism. The better room-temperature ferromagnetism is given with the higher Mn³⁺ concentration. The bound magnetic polarons (BMP) theory can be used to prove our room-temperature ferromagnetic properties. The film with the maximum concentration of Mn³⁺ presents strongest ferromagnetic signal at annealing temperature 950 °C. Higher annealing temperature (such as 1150 °C) is not proper because of the second phase Mn_xGa_y formation.     

400W行波热声发电系统的实验研究

本文阐述了为太阳能发电系统设计的400 W行波热声发电系统(TWTAEG)的实验研究过程.实验系统由行波热声发动机和直线发电机组成,系统采用平均压力为3.5 MPa的氦-氩混合气体为工质,其中氩气分压比为1.4%,系统运行频率为74Hz.实验中最大输出电功为446 W,此时的热电效率为13%;在输出电功为416 W时热...