氢化物发生-荧光光度法测定微量硒

本文提出了一个氢化物发生-荧光光度法测定微量硒的新方法。用硼氢化钾溶液将硒(Ⅵ)还原成H_2Se挥发出来,用8-羟基喹啉-5-磺酸钯溶液吸收,生成难溶的PdSe,释放出的8-羟基喳啉-5-磺酸与Al~(3+)生成发荧光的络合物,其荧光强度与硒(Ⅳ)量成正比。方法的检出限为0.26ng/ml。     

Speciation analysis of selenium enriched green onions (Allium fistulosum) by HPLC-ICP-MS

Green onions (Allium fistulosum) enriched with 10 or 100 μg mL^− 1 Se(IV) or SeMet were analyzed for total selenium and species distribution. Anion and cation exchange chromatographies were applied for the separation of selenium species with mass spectrometric detection. Two different sample preparation methods (NaOH and enzymatic) were compared from the Se extraction efficiency point of view. Total selenium concentration accumulated by the onions reached the 200 μg g^− 1 level expressed for dry weight when applying SeMet at a concentration of 100 μg mL^− 1 as the source of Se. Speciation studies revealed that both in onion bulbs and leaves the predominant form of organic selenium is Se-methyl-selenocysteine (MeSeCys). When Se(IV) was applied for Se-enrichment at a concentration level of 100 μg mL^− 1 both onion leaf and bulb contained a significant amount of inorganic selenium. An unknown compound was also detected.     

Determination of selenium, zinc and cadmium in antidandruff shampoos by atomic spectrometry after microwave assisted sample digestion

Microwave assisted pre-treatments for atomic spectrometric determination (inductive coupled plasma-optical emission spectrometry, ICP-OES or flame atomic absorption spectrometry, FAAS) of metallic elements, usually present in antidandruff shampoos, are proposed. They are based on the digestion of the sample with HNO₃ into a closed reactor, which is irradiated at 800 W for a few minutes. Selenium was determined by ICP-OES. The limit of detection was 0.11 mg l⁻¹; the relative standard deviation (R.S.D.) for the selenium content in the samples was in the 0.6–3.6% range. The results obtained were in agreement with the label contents and the recovery of the proposed method was in the 100–106% range. Zinc and cadmium were determined by FAAS. The limit of detection for zinc determination was 0.078 mg l⁻¹; the R.S.D. for zinc contents was in the 0.8–8.6% range. A limit of detection of 0.09 mg l⁻¹ was obtained for cadmium determination; the R.S.D. for cadmium contents was in the 0.7–2.7% range. The determinations were performed after two different sample mineralization pre-treatments — dry ashing (in an electric furnace) and wet mineralization (in a microwave oven). Both methodologies provided comparable results for zinc and cadmium determination in shampoos. The proposed microwave assisted digestion procedures allow a precise and accurate determination of selenium, zinc and cadmium in commercial antidandruff shampoos, and the sample pre-treatment is less time-consuming than the classic methods.     

细胞动力学研究VIII.Na2SeO3对黑根菌作用特征

The Characteristics of the action of Na2SeO3 on Rhizopus nigrocans has been studied by means of microcalorimetry, the relationship between growth rate constants and the concentration of Na2SeO3 is
k=0.03608exp[-0.003608(c+8.60)2]
It was found that Na2SeO3 of low concentration has promoting action on the growth of Rhizopus nigrocans cells, and high concentration of Na2SeO3 has inhibitory action. The study has provided a lot of information on the bioaffect of selenium and the research of toxicology.     

Synthesis of chitosan resin possessing 3,4-diamino benzoic acid moiety for the collection/concentration of arsenic and selenium in water samples and their measurement by inductively coupled plasma-mass spectrometry

A chitosan resin functionalized with 3,4-diamino benzoic acid (CCTS-DBA resin) was newly synthesized by using a cross-linked chitosan (CCTS) as base material. The adsorption behavior of trace amounts of elements on the CCTS-DBA resin was examined by the pretreatment with a mini-column and measurement of the elements by inductively coupled plasma-Mass spectrometry (ICP-MS). Arsenic(V) could be retained on the CCTS-DBA resin at pH 3 as an oxoanion of H₂AsO₄⁻. Selenium(VI) is strongly adsorbed at pH 2 and pH 3 as an oxoanion of SeO₄²⁻, while selenium(IV) as HSeO₃⁻ is adsorbed on the resin at pH 3. The sorption capacities are 82, 64, and 88 mg g⁻¹resin for As(V), Se(IV), and Se(VI), respectively. The effect of common anions and cations on the adsorption of As(V), Se(IV), and Se(VI) were studied; there was no interference from such anionic matrices as chloride, sulfate, phosphate, and nitrate up to 20 ppm, as well as from such artificial river water matrices as Na, K, Mg, and Ca after passing samples through the mini-column containing the resin. The CCTS-DBA resin was applied to the collection of arsenic and selenium species in bottled drinking water, tap water, and river water.     

Identification of selenium species in urine by ion-pairing HPLC–ICP–MS using laboratory-synthesized standards

This study focused on the detection/identification of possible selenium metabolites in human urine. Organoselenium compounds not commercially unavailable were synthesized and characterized by electrospray mass spectrometry. Separation of selenomethionine, methylselenomethionine, trimethylselonium, selenoethionine, and selenoadenosylmethionine was achieved by ion-pairing HPLC with a mobile phase of 2 mmol L^–1 hexanesulfonic acid, 0.4% acetic acid, 0.2% triethanolamine (pH 2.5), and 5% methanol. The column effluent was introduced on-line to inductively coupled plasma–mass spectrometry for selenium-specific detection (⁷⁷Se and ⁷⁸Se). For selenium speciation in urine, solid-phase extraction was carried out using C₁₈ cartridges modified with hexanesulfonic acid. Selective retention of cationic species was observed from acidified urine (perchloric acid, pH 2.0). After elution with methanol, evaporation, and dissolution in the mobile phase, the sample was introduced to the HPLC–ICP–MS system and the chromatographic peaks were assigned by adding standards. The species identified in urine were selenomethionine, trimethylselonium ion, and selenoadenosylmethionine. The last species was detected for the first time and our results suggest that selenomethionine might enter the metabolic pathway of its sulfur analog in the activated methylation cycle.Kazimierz Wrobel and Katarzyna Wrobel are on the leave from the Institute of Scientific Research, University of Guanajuato, L. de Retana No. 5, 36000 Guanajuato, Gto., Mexico     

秩消因子分析—荧光光度测定某些食物中的营养元素硒

本文应用秩消因子分析－荧光光度法测定了食物中营养元素硒的含量，与文献〔１〕报道的ＤＡＮ－荧光光度法测定结果比较，具有良好的统计学一致性，从而为简化实验操作，改善痕量硒测定的准确性和灵敏度提供了新的可能。     

Selenium speciation in foods: Preliminary results on potatoes

The present paper deals with the speciation of selenium in potatoes (enriched or not in selenium). The study was carried out by using differential pulse cathodic stripping voltammetry (DPCSV) for quantifying selenium. Results obtained provide evidence that the selenium content in the protein fraction is rather independent from the selenium added to the plants during their growth. On the contrary, the amount of Se in the non-protein fraction (water and starch) in Se-enriched sample is significantly higher than in non-enriched one, suggesting that it is the main selenium-storing site. In this fraction the Se(VI)/Se(IV) ratio seems independent from selenium application but it may be related to the redox conditions. The accumulation of selenium in the non-protein fraction is tentatively ascribed to the “Se–starch interaction” that should be able to modulate both the Se absorption into proteins and, possibly, its toxic effect for the plant itself.     

ICP—AES法测定玩具材料中痕量砷,硒,锑

用电感耦合等离子体原子发射光谱法（ＩＣＰ－ＡＥＳ０测定了玩具材料中的痕量砷，硒和锑。方法简便快速，回收率为９７．５％－１０２．７％，相对标准偏差小于３％。     

天然药物及制剂中微量元素硒的测定方法概况

硒是人体必需的微量元素，具有抗肿瘤、防衰老、防辐射和增强机体免疫力等多种功能。本文就国内近年来对天然药物及其制剂中微量元素硒的分析方法概况作一综述，包括：原子吸收分光光度法、荧光分光光度法、电感耦合等离了光谱法、催化分光光度法、分光光度法、化学发光淬灭法、极谱法、中子活化分析法和色谱法等。