Validated LC‐MS method for simultaneous quantitation of catalpol and harpagide in rat plasma: application to a comparative pharmacokinetic study in normal and diabetic rats after oral administration of Zeng‐Ye‐Decoction

A simple and efficient liquid chromatography‐mass spectrometry (LC‐MS) method was developed and validated for simultaneous quantitation of catalpol and harpagide in normal and diabetic rat plasma. Protein precipitation extraction with acetonitrile was carried out using salidroside as the internal standard (IS). The LC separation was performed on an Elite C₁₈ column (150 × 4.6 mm, 5 µm) with the mobile phase consisting of acetonitrile and water within a runtime of 12.0 min. The analytes were detected without endogenous interference in the selected ion monitoring mode with positive electrospray ionization. Calibration curves offered satisfactory linearity (r > 0.99) at linear range of 0.05–50.0 µg/mL for catalpol and 0.025–5.0 µg/mL for harpagide with the lower limits of quantitation of 0.05 and 0.025 µg/mL, respectively. Intra‐ and inter‐day precisions (RSD) were <9.4%, and accuracy (RE) was in the ?6.6 to 4.9% range. The extraction efficiencies of catalpol, harpagide and IS were all >76.5% and the matrix effects of the analytes ranged from 86.5 to 106.0%. The method was successfully applied to the pharmacokinetic study of catalpol and harpagide after oral administration of Zeng‐Ye‐Decoction to normal and diabetic rats, respectively. Copyright © 2013 John Wiley & Sons, Ltd.     

Fabrication of photoluminescent liquid crystal device using an in situ self-assembled molecular layer of a pyrene derivative

An in situ self-assembled molecular layer of 1-pyrenesulfonic acid sodium salt as an alignment agent was formed on indium tin oxide substrates for vertically aligning liquid crystals (LCs). The thus-aligned LCs exhibited uniform vertical alignment under crossed polarisers. The electro-optical characteristic of the LC cell fabricated using this method exhibited better performance than those of conventional LC cells with a polyimide alignment layer. Because the proposed alignment method is a simple one and involves low concentrations of the alignment agent (0.05 wt%), it is highly cost-effective. Further, the pyrene derivative, when mixed with LCs, exhibited photoluminescence (PL) under ultraviolet light. Given that the proposed method resulted in highly vertically aligned LCs and the alignment agent exhibited PL, the method should find wide use in the fabrication of colour-filter-free LC displays.     

Determination of limonin in dog plasma by liquid chromatography–tandem mass spectrometry and its application to a pharmacokinetic study

A highly sensitive liquid chromatography–tandem mass spectrometry method was developed and validated for the determination of limonin in beagle dog plasma using nimodipine as internal standard. The analyte and internal standard (IS) were extracted with ether followed by a rapid isocratic elution with 10 mm ammonium acetate buffer–methanol (26:74, v/v) on a C₁₈ column (150 × 2.1 mm i.d.) and subsequent analysis by mass spectrometry in the multiple reaction monitoring mode. The precursor to product ion transitions of m/z 469.4 → 229.3 and m/z 417.2 → 122.0 were used to measure the analyte and the IS. The assay was linear over the concentration range of 0.625–100 ng/mL for limonin in dog plasma. The lower limit of quantification was 0.312 ng/mL and the extraction recovery was >90.4% for limonin. The inter‐ and intra‐day precision of the method at three concentrations was less than 9.9%. The method was successfully applied to pharmacokinetic study of limonin in dogs. Copyright © 2012 John Wiley & Sons, Ltd.     

MODEL SIMULATION OF WATER-IN-OIL XANTHAN FERMENTATION

The W/O xanthan fermentation is simulated by integrating the microbial kinetic behaviors and the multiple-phase process characteristics. Model 1 assumes uniform redistribution of cells, substrates and product by frequent droplet breakup and coalescence. Model 2 simulates the system of viscous aqueous phase with minimal droplet breakup and component redistribution. The real fermentation should proceed within the bounds set by the two models. Effects of various parameters are evaluated. The aqueous-phase xanthan concentration (X_n) and volumetric productivity (Q_P) achieved at 200 h are used as the indicators. X_n and Q_P increase with nitrogen-source concentration (S_NO) initially but plateau (Model 1) or decrease slightly (Model 2) at high S_NO. X_n (at 200 h) decreases with increasing aqueous-phase volume fraction (f). Q_P, however, increases with f reflecting its basing on the total dispersion volume. Increasing agitation and aeration result in higher X_n and Q_P. The higher agitation enhances the G/O interfacial oxygen transfer and reduces the droplet size. Increasing aeration improves the G/O interfacial transfer but increases the droplet size. Its net positive effect implies a rate-limiting step at G/O interface. The W/O fermentation can produce far higher X_n (> 200 kg/m3) and Q_P( > 0.8 kg/m3-h) than the conventional fermentation (X_n ～ 50 kg/m3, Q_P ～ 0.5 kg/m3-h).     

Multiferroic characteristics of the strained epitaxial Bi0.9Ho0.1FeO3 thin film

We fabricated high quality epitaxial Bi_0.9Ho_0.1FeO₃ thin films which exhibited the tetragonally stained structure with a c/a ratio of about 1.04. The Bi_0.9Ho_0.1FeO₃ thin film showed a good ferroelectric property with the high remanent polarization (P_r) of about 80 μC/cm². The ferromagnetic hysteresis loop with a clear remanent magnetization was shown. The coercive field and the remanent magnetization of the Bi_0.9Ho_0.1FeO₃ film are 6200 Oe and 1.7 emu/g, respectively. The abrupt conduction due to space charge limited (SCL) was revealed in leakage current density versus electric field.     

Resonantly pumped Q-switched Er:GdVO4 laser

We describe a Q-switched Er:GdVO₄ laser resonantly pumped by a MgO-doped periodically poled LiNbO₃ optical parametric oscillator （MgO: PPLN OPO） at 1536 nm. In continuous-wave lasing, the maximum output power is 1.14 W with an incident pump power of 4.7 W and a slope efficiency of 27%. In Q-switched operation, 1.1 mJ of output pulse energy is achieved at 200 Hz. The upper-state lifetime at different pulse repetition frequencies is also calculated.     

基于混合吸附剂磁性固相萃取/高效液相色谱-串联质谱法测定水中磺胺和喹诺酮类抗生素残留

通过制备磁性大孔有机共聚物材料(Fe₃O₄@Si O₂@PLS)和磁性金属有机骨架材料(Fe₃O₄@ZIF-8),将两种材料同时作为磁性吸附剂,建立了混合吸附剂磁性固相萃取/高效液相色谱-串联质谱(MSPE/HPLC-MS/MS)测定水中4种磺胺类和8种喹诺酮类抗生素残留的分析方法。通过扫描电子显微镜(SEM)、傅里叶变换红外光谱(FT-IR)和X-射线衍射仪(XRD)对两种磁性材料进行表面形貌和结构表征,结果显示,亲水亲脂大孔有机共聚物(PLS)包覆于磁性纳米粒子Fe₃O₄表面,且Fe₃O₄成功附着于正六边形金属有机骨架材料(ZIF-8)晶体表面,可以满足磁性固相萃取的要求。通过优化吸附剂用量、萃取方式、吸附时间、样品p H值、洗脱剂种类及洗脱时间,在最优的实验条件下,12种目标物的线性范围为0.5～10μg/L,相关系数(r²)为0.996 1～0.999 8,检出...     

Toggle-switchable fluorescence of bisindolylmaleimide derivatives by reversible esterification/hydrolysis

Isomers based on the bisindolylmaleimide architecture were reported in this Letter. Introducing hydroxyl to this architecture lead to quenching the fluorescence of bisindolylmaleimide. The fluorescence was recovered with its hydroxyl group esterified. Ester group can be easily transformed to hydroxyl group by hydrolysis reaction. Thus, a toggle-switchable fluorescence, ‘off-on’ cycle can be established on the basis of reversible esterification/hydrolysis reaction.     

Measurement of the Binding of Adenosylcobalamin to Glutamate Mutase by Fluorescence Spectroscopy

Fluorescence spectroscopy is a fast, highly sensitive technique for investigating protein‐ligand interactions. Intrinsic protein fluorescence is usually occurred by exciting the proteins with 280‐295 nm ultraviolet light, and the light emission is observed approximately between 330‐350 nm. No emission light between 330‐350 nm can be observed when adenosylcobalamin (AdoCbl) is excited at 282 nm. The binding of AdoCbl to glutamate mutase was therefore investigated by fluorescence spectroscopy in this study. Our results show that direct measurement for determining the K_d of AdoCbl by fluorescence spectroscopy leads to significant errors. Here we report the source of error and a corrected method for measuring the binding of coenzyme B₁₂ to glutamate mutase using fluorescence spectroscopy.