Simultaneous screening for lipophilic and hydrophilic toxins in marine harmful algae using a serially coupled reversed-phase and hydrophilic interaction liquid chromatography separation system with high-resolution mass spectrometry

The presence of toxins in harmful algal blooms (HABs) poses considerable concerns because of their potential adverse effects on ecological environments and human health. When marine HABs occur, efficient screening and identification of toxins in different kinds of HAB algae remains a challenge. In this study, the applicability of serial coupling of reversed-phase liquid chromatography (RPLC) and hydrophilic interaction chromatography (HILIC) combined with high resolution mass spectrometry (HR-MS) for the simultaneous screening and identification of various kinds of known lipophilic and hydrophilic toxins in HAB algae was investigated for the first time. Ultrasound-assisted extraction (UAE) was explored to extract both lipophilic and hydrophilic toxins in algae simultaneously. As in most cases, toxin standards were not available; therefore, an identification procedure based on accurate mass data and chromatographic behavior was proposed. According to this procedure, eight known lipophilic toxins and 11 hydrophilic toxins were successfully detected in a single injection, and the proposed method was validated. Satisfactory sensitivity, repeatability (RSD <14.87%) and recovery (89.4–105.8%) of the method were achieved. A major advantage of the proposed method is that it can almost detect members of all eight groups of marine algal toxins in a single run. Using this method, several known toxins in different marine toxigenic algae including Alexandrium tamarense, Alexandrium minutum and Prorocentrum lima were successfully observed and identified. This work demonstrates that RPLC/HILIC-HR-MS combined with an accurate mass list of known marine algal toxins may be used as a powerful tool for screening of different classes of known toxins in marine harmful algae.     

糖簇分子和糖树状分子及其生物学活性

糖簇分子和糖树状分子是近年来发展起来的一类新型糖缀合物,其目的是模拟天然存在的“多元效应”。本文主要综述了目前已知糖簇分子和糖树状分子所具有的生物活性及其潜在的应用领域。     

Simultaneous detection of attomolar pathogen DNAs by Bio-MassCode mass spectrometry

A general method is described to analyze pathogen DNAs in homogenous solution by a novel Bio-MassCode probe, using a small organic (namely disulfide) "reporter mass" that self-assembled in oligonucleotide-modified gold nanoparticles. With conventional MALDI TOF MS, the assay simultaneously detected DNAs for HIV, HBV, HCV, and TP with extraordinarily high sensitivity in the low attomolar (10(-18) M) range without any other amplification.     

基于飞轮储能的并网风电场有功功率及频率控制方法研究

为平缓风电场输出,实现大规模风电并网并参与系统的频率控制,设计了一个基于永磁同步电机的飞轮储能系统,利用飞轮储能系统的快速充放电能力实现了风电场并网有功功率与一次频率控制.研究了飞轮储能系统的参考功率计算方法,根据该参考功率的变化实现储能系统充放电运行状态的转化.在Matlab/Simulink中建立了该储能系统模型,进行了风电场并网的有功功率及频率控制仿真,仿真结果表明该方法可以有效地平缓风电场的有功功率输出,参与系统的一次调频.     

Development of a quality evaluation system for Panax quinquefolium. L based on HPLC chromatographic fingerprinting of seven major ginsenosides

A HPLC fingerprinting method based on the distribution and contents of seven major ginsenosides has been developed for the quality evaluation of Panax quinquefolium. L roots cultivated in China, Singapore and Canada. The method is ideally suited for the fingerprinting of P. quinquefolium. L samples or its derived products for sample authentication or quality control, e.g. pharmaceutical stability studies. Different extraction methods have been evaluated and a protocol established to maximize the gensinosides yields in routine operations. Hierarchical clustering analysis of the fingerprints demonstrates that the distribution and contents of ginsenosides in P. quinquefolium. L root vary depending on geographic location; and the quality of Jilin-cultivated P. quinquefolium. L roots is similar in composition to Canada-cultivated ones, which are generally considered among the best quality in P. quinquefolium. L.     

ICP－AES初级专家系统中的谱线模拟

本文阐述了ＩＣＰ－ＡＥＳ初级专家系统中谱线模拟的理论基础，模拟了Ｃａ、Ｍｇ和Ａｌ在ＬＴＥ和ｎｏｎ－ＬＴＥ情况下的离子线与原子线，证明在ｎｏｎ－ＬＴＥ条件下，离子线与原子线的强度比增强了，比ＬＴＥ条件下的结果更接近实际扫描谱图。本研究模拟计算了Ｃａ和Ｍｇ离子线的跃迁上能级能量对离子线强度的影响。     

ICP-AES初级专家系统中的谱线干扰校正的研究

本工作建立了ＩＣＰ－ＡＥＳ初级专家系统中的谱线干扰校正模块，并运用于实际光谱干扰校正问题，获得较好的结果     

钯－硝酸镁基体改进剂石墨炉原子吸收光谱法测定六味地黄丸中锡

本实验建立了钯－硝酸镁基体改进剂石墨炉原子吸收光谱法测定六味地黄丸中锡的方法。研究了基体改进剂的加入方式对测定的影响。方法的相对标准偏差为２．５％，回收率在９０％～１１０％之间，检出限为０．３ｎｇ／ｍＬ。本方法可用于中成药中锡的测定。     

Simultaneous determination nucleosides in marine organisms using ultrasound-assisted extraction followed by hydrophilic interaction liquid chromatography-electrospray ionization time-of-flight mass spectrometry

A new method has been developed based on ultrasound-assisted extraction (UAE) followed by hydrophilic interaction chromatography (HILIC) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF/MS) for the simultaneous determination of 16 nucleosides and nucleobases in medicinal extracts of various marine organisms. The separation was achieved on a Venusil HILIC column (250×4.6 mm id, 5 μm) and gradient elution using a solution of acetonitrile and buffer (0.20% formic acid and 20 mmol/L ammonium acetate) as the mobile phase. Identification of the 16 target nucleosides and nucleobases was based on the retention time, UV spectra, and mass measurements of the protonated molecules ([M+H](+)) and main fragment ions (ESI-TOF/MS). In addition, non-target compounds of 2'-deoxyinosine and four other amino acids were also tentatively identified by ESI-TOF/MS. The 16 target compounds were quantified by HILIC-ESI-TOF/MS under optimized mass conditions. All calibration curves showed good linearity (r(2)>0.9951). The recoveries were 84.72-124.10%, and the limits of detection of the 16 target compounds were 0.6-130.0 ng/mL. The developed method was applied to quantify the target compounds in 15 batches of various marine organisms. The method has potential applicability for the identification and determination of highly polar and low-concentration active compounds in marine organisms.