硒酵母中硒含量测定方法的研究

报道了人工培养硒酵母中总硒、无机硒和有机硒的测定方法,建立了无机硒和有机硒的鉴别方法,并采用透析处理法使硒酵母中的无机硒和有机硒得以分离;还报道了不同培养条件下得到的5种硒酵母中总硒、无机硒和有机硒的定量分析数据,为硒酵母在医药和添加剂领域的应用提供了可靠的数据。     

Determination of elemental selenium and pyrite-selenium in sediments

A method is described for the selective determination of concentrations of elemental selenium and pyrite-selenium in sediments. A 1 M sodium sulfite solution is used to solubilize elemental selenium and a Cr(II) solution releases selenium in pyrite. The accuracy of the methods was evaluated by using various selenium compounds. The detection limits for the elemental and pyrite-selenium procedures are 0.001 and 0.025 μg Se per gram of sediment, respectively. The relative standard deviationis < 10% for elemental selenium and < 16% for pyrite-selenium. These and other procedures were used for selenium speciation in marine and freshwater sediments.     

SE-HPLC-ICP-MS联用技术在富硒蛹虫草硒蛋白形态分析中的应用研究

从富硒培养的虫草中提取可溶性蛋白质, 经过(NH4)2SO4分级盐析, 采用ICP-MS对不同盐析组分中蛋白及硒分布进行测定, 结果表明, 富硒蛹虫草的可溶性硒含量占总硒含量的69.3%以上, 在所得的各级蛋白组分中, 除A组分(0~30%饱和度的盐析)外, 其它各组分均存在含硒蛋白, 其硒含量高低顺序为B组分(30%~50%饱和度的盐析)>C组分(50%~75%饱和度的盐析)>D组分(75%~100%饱和度的盐析)>A组分. 采用SE-HPLC-ICP-MS联机技术对样品中的硒蛋白进行分离检测, 结果表明, 其分子量分布在114000和1000之间， 且含量各异. 进一步研究结果表明, 硒在虫草体内参与了蛋白的合成, 这对于以蛹虫草为载体将无机硒有机化具有重要意义.     

原子荧光法测定植物样品中的硒

研究建立了氢化物发生-原子荧光光谱法测定植物样品中硒的方法,对样品处理、干扰及消除进行了探讨。结果表明,该法的检出限为0.56ng/g,回收率为93.6%~99.2%,RSD为2.8%~5.2%。     

Heat capacity and stability of monoclinic selenium

Heat capacities of monoclinic selenium have been measured by computer interfaced differential scanning calorimetry from 100 to 379 K. Using literature data for low temperature heat capacities, enthalpies, entropies, and free enthalpies are calculated up to the zero entropy production melting temperature of 413 K. A comparison with trigonal selenium shows that there is no floor temperature for the stability of trigonal selenium. Monoclinic selenium is metastable relative to trigonal selenium at all temperatures.     

Simple method for determination of selenium in biological materials by flameless atomic-absorption spectrometry using a carbon-tube atomizer

A method for determination of selenium in biological materials by flameless atomic-absorption spectrometry using a carbon-tube atomizer is described. The sample is burned by an oxygen-flask combustion procedure, the resulting solution is treated with a cation-exchange resin to eliminate interfering cations, the selenium is extracted with dithizone in carbon tetrachloride and the resulting selenium dithizonate is combined with nickel nitrate in the carbon tube to enhance the sensitivity for selenium and avoid volatilization losses. The method measures selenium concentrations as low as 0.01 mug/g with a relative standard deviation of 8%.     

Determination of Selenium in Foodstuffs by Cathodic Stripping Voltammetry at a Mercury–Graphite Electrode

A universal procedure was developed for the voltammetric determination of total selenium in various foodstuffs. The procedure involves the mineralization of a test sample with magnesium nitrate followed by the reduction of selenium(VI) to selenium(IV) in 6 M HCl and the determination of selenium by cathodic square-wave voltammetry at a mercury–graphite electrode in an HCl solution in the presence of copper and mercury ions.     

Interference from iodide in the determination of trace level selenium

The rate of the reaction between iodide and selenium(IV) at trace levels to form selenium and iodine has been determined in 1-6M hydrochloric acid. The reaction rate increases rapidly with acidity. When hydrochloric acid is added to reduce selenate to selenite prior to the determination of total selenium, some selenium may be lost by reduction to the element if iodide is present. A table of half-lives of the selenite-iodide reaction under various conditions is presented. A method for removal of iodide is suggested.     

A chemical concentration x-ray determination of selenium in copper-, nickel-and iron-base alloys

A method is described for the determination of selenium in various metals and alloys at concentrations of 3-100ppm. A chemical separation is made by filtration after reduction of the selenious acid to elemental selenium with hydroxylamine hydrochloride. The pure selenium product is readily analysed by X-ray fluorescence; the method is free from errors due to matrix effects. The relative standard deviation is 6 % for a copper-nickel alloy at the 60 ppm level.     

Selenium speciation in animal tissues after enzymatic digestion by high-performance liquid chromatography coupled to inductively coupled plasma mass spectrometry

A procedure is described for the enzymatic digestion of tuna and mussel samples that allows the determination of selenium species by high-performance liquid chromatography in conjunction with inductively coupled plasma mass spectrometry. The species were extracted by two-step enzymatic hydrolysis with a non-specific protease (subtilisin). The selenium species were separated on a Spherisorb 5 ODS/AMINO column using two different chromatographic conditions, namely phosphate buffers at pH 2.8 and pH 6.0 as mobile phases. The method determines organic (trimethylselenonium, selenocystine, selenomethionine and selenoethionine) and inorganic selenium species (selenite and selenate), but only organic selenium species were found in the samples. The sum of identified selenium species in the sample was about 30% of the total selenium present in the enzymatic extract despite the fact that recoveries of total hydrolysed selenium were 93-102%. Trimethylselenonium ion and selenomethionine were found in both tuna and mussel samples and an unknown selenium species was also found in tuna samples.     

Determination of arsenic and selenium in steel by an X-ray technique utilizing chemical preconcentration

A chemical X-ray method is proposed for determining trace amounts of arsenic and selenium in steel. The method utilizes a prechemical separation from the iron matrix and concentration of arsenic and selenium on a micr?pore membrane by reduction to the free metal by tin(II). Selenium was found to be a suitable carrier for arsenic (300 mug of selenium for the quantitative precipitation of 10-200 mug of arsenic). Arsenic (300 mug) was found to be a suitable carrier for up to 200 mug of selenium. Up to 200 mug of tellurium and antimony were experimentally found not to be co-precipitated with either arsenic or selenium.     

TISSUE SELENIUM LEVELS AND GROWTH RESPONSES OF MICE FED SELENOMETHIONINE,SE-METHYLSELENOCYSTEINE OR SODIUM SELENITE

Abstract

Mice fed diets containing selenomethionine at a level of 20 ppm selenium and raised to 30 ppm selenium at 3 weeks on experiment showed (1) delayed response to selenium toxicity, (2) slow recovery from the toxicity after removal of selenium from the diet and (3) relatively high deposition and retention of tissue selenium. These data suggest that selenomethonine initially becomes incorporated in to the primary structure of proteins and as such is not particularly toxic. However, upon its slow removal from protein, selenomethionine becomes toxic by forming selenium IV compounds through a pathway similar to that followed by methionine.

Mice fed diets containing sodium selenite or Se-methylselenocysteine at the same level of selenium as the selenomethionine diet showed (1) immediate response to selenium toxicity (2) rapid recovery from the toxicity after removal of selenium from the diet and (3) relatively low deposition and relatively rapid depletion of tissue selenium. These data suggest that sodium selenite and Se-methylselenocysteine ultimately follow similar metabolic pathways and do not become part of the primary structure of proteins. A possible metabolic route for Se-methylselenocysteine is that it is oxidized to toxic selenium IV compounds through an oxidative pathway similar to that followed by S-methylcysteine.     

离子缔合物二级散射光谱的分析应用: 硒(IV)-碘化物-罗丹明B体系

从硒(IV)-碘化物-罗丹明B反应体系的研究中, 发现了离子缔合物水溶液的两种二级散射光谱现象。研究了它们的光谱特征、影响因素和适宜条件, 确定了二级散射强度与溶液中离子缔合物浓度的关系, 提出了利用二级散射光谱测定痕量硒的高灵敏分析方法。对反应机理和二级散射变化的原因也进行了初步的探讨。     

硒与心血管疾病

介绍了硒的生物学特征及与心血管疾病的关系,包括：硒的生物学特征及作用,硒与自由基,硒与动脉粥样硬化,硒与冠心病,硒与克山病.     

Determination of selenium in drugs by oxygen flask combustion and ion chromatography

A method is described for the determination of trace selenium (impurities in medicinal organic compounds) by ion chromatography (IC) after oxygen flask combustion. All selenium compounds formed by oxygen flask combustion are converted to selenate ion by heating with nitric acid and potassium permanganate. The selenate ion is then determined by IC, using a simple recycle system to eliminate interfering ions. The detection limit of selenium is 0.4 nmol in 50 mg of sample. The recoveries of selenium added to seven drugs are ca. 95-103% with relative standard deviations of 1-6%.     

氢化物发生-原子荧光光谱法(HG-AFS)测定特硬铅合金中硒和碲

建立了氢化物发生-原子荧光光谱法(HG-AFS)测定特硬铅合金中硒和碲的分析方法。试样经硝酸和酒石酸溶解,硫酸沉淀分离基体铅元素。移取部分试液,在40%盐酸介质中直接用氢化物发生-原子荧光光谱法(HG-AFS)测定样品中的硒;另移取部分试液,加入氢溴酸挥发除去砷、锑、锡、硒等元素,在40%盐酸介质中用氢化物发生-原子荧光光谱法(HG-AFS)测定样品中的碲。考察了测定的最佳条件、铅及共存元素对测定的影响。测定硒和碲的相对标准偏差分别为7.5%～9.3%和3.6%～13.0%,加标回收率分别为88%～92%和98%～102%。准确度和精密度均能满足分析需要,具有较强的实用性。     

The gas chromatographic determination of selenium(IV) and total selenium in natural waters with 1,2-diamino-3,5-dibromobenzene

The total selenium and selenium(IV) contents in sea water and river water can be determined directly by a gas chromatographic method with l,2-diamino-3,5-dibromobenzene without preconcentration. The reagent reacts only with selenium(IV) to form a 4,6-dibromopiazselenol; other oxidation states of selenium must therefore be converted to the tetravalent state for total selenium determinations. The piazselenol formed can be extracted quantitatively into 1 ml of toluene from 500 ml of sample water. A method is proposed for the determination of selenium(IV) and total selenium in natural waters at levels as low as 2 ng l^-1. Coastal sea water and river water in Japan contain 8–30 ng of Se(IV) and 20–50 ng of total Se per liter.     

The determination of selenium in urine

The selenium excreted in urine can be measured to assess the dietary status of selenium, an essential trace element in human nutrition. The objectives of this work were: 1) to develop a procedure, capable of high sample throughout, by which the major interferences can be reduced such that selenium concentrations can be measured in urine by Neutron Activation Analysis (NAA) using^77mSe (17.4 s; and 2) to apply the method to a human dietary selenium study in which several selenium monitors were compared. The method involves a pre-irradiation arsenic-coprecipitation separation of the selenium from urine in the presence of a high specific-activity⁷⁵Se tracer. The processed urine samples are analyzed using NAA. The procedure was applied to 58 urine specimens longitudinally collected from 12 subjects consuming three different levels of selenium. A dose-response relationship was observed in urine as well as a high correlations with both serum and whole blood selenium concentrations.     

HPLC-ICP-MS联用技术在富硒金针菇硒的形态分析中的应用

从富硒培养的金针菇中分离得到含硒化合物, 并采用SE-HPLC-ICP-MS联机技术对浸提液中的含硒化合物进行分离分析; 同时对样品中的硒蛋白在特定条件下水解, 采用RP-HPLC-ICP-MS联机技术对水解液中硒代氨基酸进行确认, 并测定其中硒的含量. 结果表明, 可溶态硒是富硒金针菇中硒的主要存在形式, 其中小分子含硒有机化合物中的含硒量占浸提液中硒的71.87%; 而含硒蛋白所占比例为4.88%; 进一步确定富硒金针菇中含有硒代胱氨酸、硒代蛋氨酸和由二者组成的含硒多肽等, 各形态硒的含量为总硒量的12.3%, 17.6%和36.8%. 本方法将具有高效分离能力的色谱技术与高灵敏度的元素检测技术成功结合, 用于含硒生物分子中硒的在线分析, 具有快速、灵敏及准确等特点.     

富硒酵母的研究开发与应用

介绍了硒的生理功能、人体对硒的需求、富硒酵母的开发以及作为功能性食品基料在各方面的应用。