Separation and purification of two minor typical diarrhetic shellfish poisoning toxins from harmful marine microalgae via combined liquid chromatography with mass spectrometric detection

A novel method was developed for the purification of two typical diarrhetic shellfish poisoning toxins from toxin‐producing marine microalgae using macroporous resin, high‐speed countercurrent chromatography–mass spectrometry, and semipreparative high‐performance liquid chromatography–mass spectrometry. Analytical high‐performance liquid chromatography–mass spectrometry was used for identification and purity analysis of okadaic acid and dinophysistoxin‐1 because they exhibit no visible or ultraviolet absorption. First, four kinds of macroporous resins were investigated, and HP‐20 macroporous resin was selected for the preenrichment and cleanup of the two target toxins. Second, the resin‐purified sample was further purified using high‐speed countercurrent chromatography coupled with a mass spectrometer. The purities of the obtained okadaic acid and dinophysistoxin‐1 were 89.0 and 83.0%, respectively, as determined through analytical high‐performance liquid chromatography–mass spectrometry. Finally, further purification was carried out using semipreparative high‐performance liquid chromatography with mass spectrometry, and the purities of the final okadaic acid and dinophysistoxin‐1 products were both over 98.0% based on the analytical high‐performance liquid chromatography–mass spectrometry chromatograms and fraction spectra. This work demonstrates that the proposed purification process is a powerful method for the preparation of high‐purity okadaic acid and dinophysistoxin‐1 from toxin‐producing marine microalgae. Moreover, it is particularly important for the purification and preparation of minor toxins that exhibit no visible or ultraviolet absorption from harmful marine algae.     

基于自动磁珠转运的转基因蛋白Cry1Ab检测

基于自动磁珠转运,建立了转基因蛋白Cry1Ab免疫检测的新方法.利用水热法制备了粒径约400 nm的纳米磁球,并进行电镜表征,通过溶胶法对磁球表面进行氨基修饰,采用戊二醛偶联对磁珠实现抗体包被,在核酸提取仪中进行酶联免疫反应,采用分光光度法进行检测.本方法对转基因蛋白Cry1Ab的检出限低于1 μg/L,与商品化酶联免...     

ASE/GC-MS法同时测定海洋沉积物中65种多氯联苯、多环芳烃与有机氯农药

建立了加速溶剂萃取/气相色谱-质谱法(ASE/GC-MS)同时测定海洋沉积物中28种多氯联苯(PCBs)、16种多环芳烃(PAHs)和21种有机氯农药(OCPs)的分析方法.结果表明,ASE的最佳萃取温度为100 ℃,最佳静态时间为5 min.GC-MS同时分析65种化合物时,PAHs的线性范围为0.05 ～5.00 ...     

无毒海洋防污剂研究进展

综述了无毒海洋防污剂研究进展,从防污活性、机理、特点及应用等方面着手介绍了近年来开发的几种新型无毒天然产物防污剂和人工合成防污剂,并就其发展前景进行了展望;指出开发研制无毒海洋防污剂是海洋防污技术的发展方向之一.     

NMR Analysis of a Complex Spin System from a Siruo-Chamigrene

The compound 2,10-dibromo-3-chloro-8-hydroxy-β-chamigrene was analysed in detail by NMR Spectroscopy. the complete assignment of the signals in the ¹H and ¹³C NMR spectra and the determination of the relative configurations were achieved by 2D NMR techniques, AM1 data and ¹H spectrum simulation. Comparisons of the results with related spiro chamigrene systems are also presented.     

Allometric scaling laws of metabolism

One of the most pervasive laws in biology is the allometric scaling, whereby a biological variable Y is related to the mass M of the organism by a power law, Y=Y₀M^b, where b is the so-called allometric exponent. The origin of these power laws is still a matter of dispute mainly because biological laws, in general, do not follow from physical ones in a simple manner. In this work, we review the interspecific allometry of metabolic rates, where recent progress in the understanding of the interplay between geometrical, physical and biological constraints has been achieved.

For many years, it was a universal belief that the basal metabolic rate (BMR) of all organisms is described by Kleiber's law (allometric exponent b=3/4). A few years ago, a theoretical basis for this law was proposed, based on a resource distribution network common to all organisms. Nevertheless, the 3/4-law has been questioned recently. First, there is an ongoing debate as to whether the empirical value of b is 3/4 or 2/3, or even nonuniversal. Second, some mathematical and conceptual errors were found these network models, weakening the proposed theoretical arguments. Another pertinent observation is that the maximal aerobically sustained metabolic rate of endotherms scales with an exponent larger than that of BMR. Here we present a critical discussion of the theoretical models proposed to explain the scaling of metabolic rates, and compare the predicted exponents with a review of the experimental literature. Our main conclusion is that although there is not a universal exponent, it should be possible to develop a unified theory for the common origin of the allometric scaling laws of metabolism.     

A Novel Nano-Sensor Based on Rhodamine-β-Isothiocyanate – Doped Silica Nanoparticle for pH Measurement

A novel and simple enzymatic method for the determination of trace cyanide in marine fish is presented. This method is based on the conversion of metal-cyanide complexes by a fungal enzyme extract containing cyanide hydratase (E.C. 4.2.1.66; CyHT) and formamidase (E.C. 3.5.1.49) into formate and ammonia. The formate produced in the sample pretreated with the fungal enzymes was measured by adding formate dehydrogenase (E.C. 1.2.1.2; FDH) and excess NAD⁺. The NADH formed accordingly was monitored at 340nm. The cyanide calibration curve was found to be linear in the range of 10–100µM, and the detection limit was 1.1µM (0.0286ppm). The proposed biotest was successfully applied to the determination of trace cyanide in a tropical marine food fish species (Russells Snapper (Lutjamus russellii)) which had been exposed to cyanide.     

Treatment of Red Tide in Ocean Using Non-Thermal Plasma Based Advanced Oxidation Technology*

A Pilot-scale experiment for the treatment of red tide in the enclosure was done in sea area of Shandong Province, P.R. China on Aug. 25, 2002. With the method of micro-gap discharge, O₂ in air and H₂O in seawater are ionized and dissociated into large numbers of OH^• radicals, and then dissolved into a part of seawater to form OH^• solution of high concentration. With OH^• concentration of 0.68 mg/L, the kill efficiencies of 29 kinds of red tide organisms such as Chaetoceros lorenzianus and so on reached 99.89%, in which bacterium and vibrio were reduced below the detection limit, also Gonyaulax cysts and Prei. Cysts with the crust were done the lowest limit of test. At the same time, the content of chlorophyll-a was decreased below the detection limit. DO (dissolved oxygen) saturation of seawater was greatly increased to 100% because the residual OH^• radical was decomposed into H₂O and O₂ after 20 min. Therefore the treatment of red tide using OH^• radicals is a kind of advanced oxidation technology, which realizes zero pollution, zero emission and zero residual in the process of the production of OH^• radicals and the treatment of red tide.*Key project of National Foundation Research from Science and Technology Ministry of China, (2002CCC00900); key project of National Natural Science Foundation of China (NSFC; 60031001).