Two new β-carboline-type alkaloids from Stellaria dichotoma var.lanceolata

Two new β-carboline-type alkaloids,dichotomine K(1) and dichotomine L(2),were isolated from the roots of Chinese medicinal plant Stellaria dichotoma L.var.lanceolata Bge.Structures of 1 and 2 were determined on the basis of chemical and spectroscopic means.     

Broadband and high efficiency metal multi-layer dielectric grating based on non-quarter-wave coatings as a reflective mirror

This article deals with designing a broadband and high efficiency metal multi-layer dielectric grating (MMDG) used to compress and stretch an ultrashort laser pulse. The diffraction characteristics of the MMDG are analysed by using the rigorous coupled-wave method. The multi-layer dielectric used as the reflective mirror is made up of non- quarter-wave coatings. Taking the diffraction efficiency of the 1 order as the value of merit function, the parameters such as groove depth, residual thickness, duty cycle, and reflective mirror are optimized to obtain broadband and high diffraction efficiency. The optimized MMDG shows an ultra-broadband working spectrum with the average efficiency exceeding 97% over 160 nm wavelength centred at 1053 nm and TE polarization. The optimized MMDG should be useful for chirped pulse amplification.     

N-3烷基取代嘧啶及其衍生物的合成

在室温条件下,经过三步反应,合成了一系列N-3烷基取代的嘧啶类化合物.该方法具有条件温和、操作简便、反应时间短、产率高等特点.目标产物经过了1HNMR,13C NMR和MS确证表征.     

A colormetric and fluorescent chemosensor for adenosine-5′-triphosphate based on rhodamine derivative

A rhodamine spirolactam derivative (1) was developed as a colormetric and fluorescent chemosensor for adenosine-5′-triphosphate (ATP) via hydrogen bonds interaction. As far as we know, this is the first case to explore ATP-induced ring-opening of spirolactam in rhodamine derivatives. It exhibited a highly sensitive “turn-on” fluorescent response toward ATP with a 47-fold fluorescence intensity enhancement under 20 equiv. of ATP added. The chemosensor can be applied to the quantification of ATP with a linear range covering from 1.0 × 10⁻⁷ to 2.0 × 10⁻⁴ M and a detection limit of 2.5 × 10⁻⁸ M. The experiment results show that the response behavior of 1 toward ATP is pH independent in medium condition (pH 6.0–8.0). Most importantly, the novel chemosensor has well solved the problem of serious interferences from other nucleoside polyphosphates such as ADP and AMP generally met by previously reported typical fluorescent chemosensors for ATP. Moreover, the response of the chemosensor toward ATP is fast (response time less than 3 min). In addition, the chemosensor can be used for the fluorescence assay for protein kinase activity with satisfactory results. The chemosensor for ATP based on hydrogen bonds interaction provided a novel strategy for the design of colormetric and ratiometric fluorescent probes for other target anions with high sensitivity and selectivity.     

Development of a sensitive and reliable high performance liquid chromatography method with fluorescence detection for high-throughput analysis of multi-class mycotoxins in Coix seed

As an edible and medicinal plant, Coix seed is readily contaminated by more than one group of mycotoxins resulting in potential risk to human health. A reliable and sensitive method has been developed to determine seven mycotoxins (aflatoxins B₁, B₂, G₁, G₂, zearalenone, α-zearalenol, and β-zearalenol) simultaneously in 10 batches of Coix seed marketed in China. The method is based on a rapid ultrasound-assisted solid–liquid extraction (USLE) using methanol/water (80/20) followed by immunoaffinity column (IAC) clean-up, on-line photochemical derivatization (PCD), and high performance liquid chromatography coupled with fluorescence detection (HPLC-FLD). Careful optimization of extraction, clean-up, separation and detection conditions was accomplished to increase sample throughput and to attain rapid separation and sensitive detection. Method validation was performed by analyzing samples spiked at three different concentrations for the seven mycotoxins. Recoveries were from 73.5% to 107.3%, with relative standard deviations (RSDs) lower than 7.7%. The intra- and inter-day precisions, expressed as RSDs, were lower than 4% for all studied analytes. Limits of detection and quantification ranged from 0.01 to 50.2 μg kg⁻¹, and from 0.04 to 125.5 μg kg⁻¹, respectively, which were below the tolerance levels for mycotoxins set by the European Union. Samples that tested positive were further analyzed by HPLC tandem electrospray ionization mass spectrometry for confirmatory purposes. This is the first application of USLE-IAC-HPLC-PCD-FLD for detecting the occurrence of multi-class mycotoxins in Coix seed.     

Polycondensation of Sebacic Acid with Primary and Secondary Hydroxyl Groups Containing Diols Catalyzed by Candida antarctica Lipase B

Abstract

The aliphatic polyesters are normally synthesized by ester interchange reactions or direct esterification of hydroxyacids or diacid/diol combinations. Biotransformation, utilizing the enzymes as catalysts, was accepted as an alternative route for the synthesis of aliphatic polyesters and offers various advantages compared with the conventional, metal-catalyzed polymerization reactions. Previous studies indicated that lipase-catalyzed polycondensation reactions between diols and diacids occurred preferentially at primary hydroxyl groups of diols, when diols contained both primary and secondary hydroxyl groups. In this work, we investigated lipase-catalyzed polycondensation of diacids and secondary hydroxyl group–containing diols, and successfully synthesized polyesters by polycondensation with secondary hydroxyl groups as well as primary hydroxyl groups. Various diols, glycerol, 1,2-propanediol, 1,3-butanediol, 2,3-butanediol, and 2,4-pentanediol were tested for the polycondensation. The polymerization was achieved by heating a mixture of lipase B, sebacic acid, and the diols in anhydrous toluene at 100 °C for 72 h. The resulting polymers were characterized by ¹H and ¹³C NMR spectroscopy, Fourier transform–infrared spectroscopy, thermogravimetric analysis, and gel permeation chromatography.