Comparison of different buffer systems for separation of 15 nucleosides by capillary electrophoresis

对毛细管电泳法分离15种核苷类化合物所用的不同缓冲液体系进行了系统比较,确定不同模式毛细管电泳法分析多种核苷类化合物的最适合背景缓冲液体系(bgE)。分别以四硼酸钠、磷酸氢二钠、乙酸钠、碳酸氢钠、乙酸铵和乙二胺(dEA)为背景电解质,对毛细管区带电泳(CzE)、毛细管电泳-电喷雾飞行时间质谱(CE-ESI-TOf/MS)以及胶束电动毛细管电泳(MEkC)3种模式进行比较,并对其中几种优势缓冲体系进行了优化。结果表明,CzE模式下使用四硼酸钠和磷酸氢二钠缓冲体系无法同时分离15种核苷类化合物,因此只适用于分析核苷类化合物数量较少的样品。而使用含有2%丙酮的300 MMOl/l dEA能完全分开15种核苷类化合物,且分辨率和峰形良好。MEkC模式下,以25 MMOl/l磷酸氢二钠(添加70 MMOl/l十二烷基磺酸钠(SdS))为缓冲盐的分离结果最佳,并且此方法能成功应用于海洋生物海葵中核苷类化合物的分离。CE-ESI-TOf/MS分析中,以20 MMOl/l乙酸铵(PH 10.0)为背景电解质,正离子模式检测,15种核苷类化合物的质谱信号均良好,检测灵敏度明显优于文献中报道的使用dEA缓冲体系的结果。本研究阐明了不同缓冲体系对15种核苷类化合物分离的适用性,为毛细管电泳技术在复杂基质中多种核苷类化合物的分离方法中的应用奠定了基础。The most suitable background electrolytes(BGEs) for simultaneous separation of 15 nucleosides by different modes of capillary electrophoresis(CE) were obtained.Various modes of CE were performed including capillary zone electrophoresis(CZE),capillary electrophoresis-electrospray ionization-time of flight mass spectrometry(CE-ESI-Tof/MS) and micellar electrokinetic chromatography(MEKC).The electrolyte buffers using sodium tetraborate decahydrate,disodium hydrogen phosphate,sodium acetate,sodium bicarbonate,ammonium acetate or 1,2-diamino-ethane(DEA) were tested,and the best of them were systematically optimized.In CZE mode,the nucleosides could not be separated completely with sodium tetraborate decahydrate or disodium hydrogen phosphate as BGEs,demonstrating the limited applicability of the two buffer systems for complex samples.However,with 300 mmol/L DEA(containing 2% acetone) as BGE,15 nucleosides could be separated with good resolution and peak shape,which proved that the DEA buffer was most suitable in CZE.The best buffer system in MEKC mode was 25 mmol/L disodium hydrogen phosphate with 70 mmol/L sodium dodecyl sulfate(SDS),and it was successfully applied for the separation of the nucleosides in Chinese Anthopleura lanthogrammica Berkly.The optimum buffer system for CE-ESI-Tof/MS analysis was 20 mmol/L ammonium acetate(pH 10.0).In the positive ion mode,the MS signals of each compound were better than those in the literature using DEA as BGE.The results of this study demonstrated the applicability of different buffer systems for the simultaneous separation of 15 nucleosides,and were helpful for the development of CE method in complex sample separation.国家自然科学基金项目(20905017);海洋公益性行业科研专项项目(201005034-3);海洋局青年基金项目(2010140);海洋一所基本科研业务专项项目(2010G25);中国科学院实验海洋生物学重点实验室开放基金课

Primary Exploration on Quality Evaluation of Holothurian Sold on the Market by HPLC Fingerprint

以10批不同产地刺参HPlC指纹图谱中的6个共有峰为评价指标,结合相似度分析,对不同刺参质量进行评价和检验。结果表明:不同批次刺参样品的6个色谱峰在指纹图谱分析过程中色谱行为相同,峰面积大,特征性强,能反映刺参的固有化学特征。结合相似度分析,可用于刺参质量评价。An optimized high performance liquid chromatography (HPLC) method was developed for the analysis of holothurian and the HPLC fingerprint was established from 10 batches of the holothurians from different habitats.The HPLC fingerprint showing 6 common characteristic peaks was used to explore the quality evaluation of holothurian and distinguish from the fakes with the similarity analysis.This method is accurate and reliable,providing a scientific basis for the quality control of holothurian and can be used to evaluate the quality of holothurian sold on the market.我国近海海洋综合调查与评价908专项(908-02-05-04):海洋药用生物资源评价和《中华海洋本草》编纂;海洋一所基本科研业务专项(GY-022008T32):海洋绿藻活性成分分析、鉴

酸雨胁迫及稀土农用条件下菠菜及其土壤中稀土元素的赋存

利用盆栽实验研究了酸雨胁迫、稀土农用条件下 ,菠菜及其土壤中稀土元素的含量及分布特征。结果表明 :菠菜地上部分的REE含量为 0 .5 2 7～ 0 .696μg·g- 1 之间 ,地下部 2 .668～ 3 .0 0 3 μg·g- 1 。土壤 2 2 9.0 9～ 2 5 0 .3 μg·g- 1 。酸雨明显地影响作物对REE的吸收和利用 ,酸度越大 ,影响越明显。随着酸雨酸度的增大、植株体内、土壤中的REE受淋洗的作用加强而表现出REE的总量随着pH的减小而逐渐减少。施用稀土后 ,植株的地上或地下部分及其土壤中的REE含量均与对照的土壤中的REE分配模式基本相同 ,遵循稀土元素分布丰度的奇偶 (Oddo Harkins)规则、轻稀土富集 ,Eu弱负异常 ,富铈配分型 ,表明稀土元素仍然主要来自土壤并受其影响

Accumulation of Rare Earth Elements in Spinach and Soil under Condition of Using REE and Acid Rain Stress

The content and distribution characteristics of REE in spinach and soil under using REE and acid rain stress were studied by pot experiments. The results show that the content of REE is 0.527～0.696 (μg·g - 1) in the above2ground portion of spinach , 21668～31003 (μg·g - 1) in the under2ground portion of spinach and 229109～ 250130 (μg·g - 1) in the soil . With the acidity of acid rain increasing , the leaching of REE in plants and soil is strengthened and the amount of REE reduces with decreasing of pH value . After REE are used , though plants show the selective absorption to Ce group elements (especially spraying on leaves) , regardless under acid rain stress or using REE or not , the distribution model of REE in the above2ground and under2ground portion of plants is basical2 ly the same with the control . Plants also follow the Oddo2Harkins rule of the REE of distribution abundance , light rare earth elements is enriched , the minus of Eu is abnormal and admeasure of Ce is a rich model . The results show that REE in plants mainly come from soil and are affected by it

Survey on Coccdia of Domestic Geese and Their Experimental Infections

作者简介: 戴亚斌( 1964- ) , 博士后, 研究员. 现在中国 农业科学院家禽研究所工作.[中文文摘]对江苏省扬州、盐城地区的鹅球虫种类进行了调查和人工感染试验.结果表明,鹅球虫感染率为74.4%.共鉴定出6种球虫,即:Eimeriaanseris、E.fulva、E.hermani、E.nocens、E.stigmosa、Tyzzeriaparvula.12日龄无球虫感染仔鹅感染5×104个混合卵囊即发生死亡.通过单种卵囊接种试验获得了5种球虫的纯种卵囊并对它们的一些生物学特征进行了观察,为这些球虫的生活史和致病性研究奠定了基础.[英文文摘]A survey of goose coccidia in the areas of Yangzhou and Yancheng, Jiangsu and their experimental infections were carried out. The results showed that coccidian oocysts were found in 74.4% of 86 faeces samples from 16 goose flocks. Six species of coccidia, Eimeria anseris, E. fulva, E. hermani, E. nocens,E. stigmosa and Tyzzeria parvula were identified. In the experiments of artificial infection three of four 12-day-old coccidia-free goslings were died after inoculated with mix oocysts of 5×10~4. Pure oocysts of 5 Eimeria species were obtained then, respectively, laying the basis for studies of their life cycles and pathog enicity

棕色固氮菌钼铁蛋白结晶及一些物理化学性质

获得了棕色固氮菌固氮酶钼铁蛋白的针状结晶,大小为2-2.5×25-65微米,成晶所要求的条件不是很严格的。SDS 电泳和氨基酸分析结果表明,钼铁蛋白分子量为250,000。只观察到一种类型亚单位。其中酸性氨基酸占优势。分子氧使针状晶体演变为发状晶丝,晶丝又密集成束。晶束可保存较长时间。氧使钼铁蛋白在电泳时形成高聚合态