氢化物发生-原子荧光光谱法测定富硒发芽糙米中的硒含量

对氢化物发生-原子荧光光谱法(HG-AFS)测定富硒发芽糙米硒含量的方法.研究表明:其检出限为0.2μg/L,相对标准偏差RSD为0.94%,平均回收率为99.74%,精密度高、稳定性好、简便快速,适合于富硒发芽糙米中硒的定量分析.通过测定采用不同浓度亚硒酸钠溶液富硒处理的发芽糙米的总硒、有机硒和无机硒含量,确定选择硒浓度为50 mg/L的溶液富硒处理后的发芽糙米品质较好.     

富硒大米中硒形态分析

采用原子荧光光度法分析了天然富硒大米中硒的主要赋存形态、分布及含量.本实验中,硒的检测线性范围为4 μg/L～20μg/L,相关系数是r=0.999 3,总硒测定的相对标准偏差(RSD)为0.966％(n=6),总硒的加标回收率为103.12％.实验表明富硒大米中的总硒含量为206.708 μg/kg,达到60 μg/kg～300 μg/kg的富硒标准,而硒主要以对人体有益的有机硒形态存在,含量为168.875 μg/kg,占总硒的81.70％,而有机硒中最主要的赋存形态是蛋白硒,含量90.170 μg/kg,占53.40％,其次多糖硒占9.28％,RNA硒占1.86％,其它形态的有机硒占35.46％.     

高效液相色谱-电感耦合等离子体质谱联用技术测定富硒食品中无机硒和有机硒的含量

目的建立高效液相色谱-电感耦合等离子体质谱联用技术(HPLC-ICP/MS)测定富硒食品中无机硒和有机硒含量的方法。方法采用纯水提取富硒食品中的无机硒,通过透析作用分离小分子量的硒化合物与样品基体,利用阴离子交换色谱分离,采用Hamilton PRP-X100分析柱和预柱(250 mm×4 mm,10μm),流动相为5 mmol/L柠檬酸铵中加2%甲醇,电感耦合等离子体质谱仪测定样品中无机硒的含量。根据总硒与无机硒的差值计算有机硒含量。结果硒(IV)和硒(VI)检出限分别为6.67和9.95μg/kg,二者回收率分别为70.2%~108.1%和73.2%~116.9%。结论该方法可满足富硒食品中无机硒和有机硒含量的测定。     

HG-AFS测定保健品及富硒食品中的硒

建立了测定硒的方法.采用微波消解氢化物发生-原子荧光法(HG-AFS)测定灵芝孢子粉、超微硒粉及富硒大米中的硒.方法的检出限为3 ng,线性范围为0.01 μg～0.2μg,平均回收率在87.5%～101.2%之间(n=5).     

叶面喷施硒肥对小麦籽粒及面粉硒含量的影响

<正>为了探明叶面喷施硒肥对小麦籽粒及制粉各粉路硒含量的影响,本研究选用4个小麦品种,在拔节和抽穗期分2次喷施0.017%亚硒酸钠叶面肥,并对成熟期籽粒进行制粉,分析各粉路的总硒、无机硒和有机硒含量。结果表明,叶面喷硒对小麦籽粒和面粉的总硒、有机硒和无机硒含量的影响存在品种间差异。喷施硒肥后,4个小麦品种籽粒的总硒     

电感耦合等离子体-质谱法与氢化物原子荧光法 测定小麦中总硒含量的方法比较

目的比较分析电感耦合等离子体-质谱法与氢化物原子荧光法测定小麦中硒含量。方法用氢化物原子荧光法(hydride generation-atomic fluorescence spectrometry,HG-AFS)和电感耦合等离子体-质谱法(inductively coupled plasma-mass spectrometry,ICP-MS)两种方法测定小麦样品中硒的含量,从检出限(LOD)、精密度(RSD)及回收率等方面进行方法学考察,其中前者采用微波消解后需继续用电热板加热消解,并加入盐酸将六价硒还原为四价硒的前处理方法,后者采用仅采用微波消解的前处理方法。结果 HG-AFS法的LOD为0.016μg/L,RSD为1.00%,回收率为94.0%~110.5%;ICP-MS法的LOD为0.028μg/L,RSD为4.06%,回收率为89.0%~116.6%。结论两种方法检测结果基本一致,均可以准确、灵敏地检测小麦样品中硒的含量。     

氢化物-原子荧光光谱法测定鸡蛋中的硒

建立了测定鸡蛋中总硒和有机硒的方法,蛋清通过三氯乙酸沉淀脱除蛋白,蛋黄通过聚乙二醇脱脂、三氯乙酸沉淀脱除蛋白后,经微波消解后直接测定鸡蛋中总硒和有机硒含量。结果表明,富硒鸡蛋样品中硒主要以有机硒形态存在,通过3%聚乙二醇脱脂, 15%三氯乙酸沉淀蛋白,可实现有机硒与无机硒的有效分离,该方法线性范围在0～20μg/g之间,无机硒检出限为0.002μg/g,方法加样平均回收率为81.6%～86.3%,相对标准偏差(rSD, n=3)为0.64%～2.6%。该方法操作简单、灵敏度高、回收率好,适合富硒鸡蛋总硒和有机硒的测定。     

富硒蛹虫草中有机硒的分析

建立高分辨-连续光源石墨炉原子吸收光谱法(high resolution-continuum source graphite furnace atomic absorption spectrophotometry,HR-CS GFAAS)测定富硒蛹虫草中有机硒的方法。参照DBS42/002-2014《湖北省食品安全地方标准富有机硒食品硒含量要求》制备富硒蛹虫草总硒测定试样,参照GB 1903.21-2016《食品安全国家标准食品营养强化剂富硒酵母》制备富硒蛹虫草无机硒测定试样,再使用HR-CS GFAAS测定富硒蛹虫草总硒和无机硒。试验以Pd(NO_3)_2(1 g/L)和Mg(NO_3)_2(0.5 g/L)混合溶液为基体改进剂,通过试验优化出基体改进剂最佳添加体积为5μL,最佳灰化温度为1 100℃,最佳原子化温度为2 200℃。测定结果表明,富硒蛹虫草总硒含量为1.407 mg/g,无机硒含量为0.083 mg/g,计算出有机硒含量为1.324 mg/g,所占百分比为94.1%,这说明富硒蛹虫草含有丰富的有机硒,是补硒良品。总硒和无机硒的加标回收率分别为95.7%和94.0%,相对标准偏差4.5%。该方法快速、准确、稳定,具有较高的实用价值,为分析食品中微量元素含量及其形态提供科学依据。     

沧州不同产地小枣中有机硒和无机硒的含量测定及差异分析

目的建立小枣中有机硒和无机硒的测定方法。方法分别利用微波消解和80%乙醇溶液提取枣样,采用氢化物发生原子荧光光谱法(HG-AFS)测定总硒和无机硒的含量,差值即为有机硒。结果硒的线性范围为0~100 ppb,检出限为0.0904 ppb,回收率94%~104%。结论通过测定沧州4个不同产地20份小枣总硒、无机硒及有机硒含量,并采用方差分析,表明4个不同产地的小枣总硒含量、无机硒及有机硒含量差异有统计学意义,其中任丘和黄骅枣中不仅总硒含量高,且有机硒含量比例也最大。     

施硒方式对葡萄吸收转化硒的影响

在温克葡萄植株生长发育阶段采取喷施和淋施2种方式施用瓜果型锌硒葆叶面肥生产富硒葡萄的应用效果。以灵川县优势果品温克葡萄为材料,在温克葡萄上喷施和淋施富含硒源的叶面肥,增加温克葡萄果实内硒的含量,探讨葡萄应用外源硒肥富硒的效果。     

The effect of juice clarification, static or rotary fermentation and fining on ochratoxin A in wine

Semillon and Shiraz grapes containing ochratoxin A (OA) were produced by inoculation of bunches on the vine with Aspergillus carbonarius . Small scale vinification of these grapes was performed and the OA content at various stages was analysed. Semillon must was treated with pectolytic enzymes and the juice after pressing was fined with bentonite. Neither pectolytic enzymes nor bentonite influenced the OA content of the clarified juice. Shiraz must was vinified by either static or rotary fermentation. No differences in the OA content of wine after pressing were noted. OA was concentrated in juice lees and gross lees. However, additional juice or wine recovered from lees after centrifugation did not display increased OA contamination compared to racked juice or wine. Addition of bentonite at 2.5 g/L to a Semillon wine containing 56 mg grape-derived protein/L and ca. 8 μg OA/kg resulted in a 67% reduction in OA concentration. Potassium caseinate showed some effect, whereas gelatin, isinglass and PVPP did not significantly diminish OA in white wine compared to wine settled without fining agents. Addition of yeast hulls at 5.0 g/L to a Shiraz wine containing ca. 5 μg OA/kg yielded a 43% reduction. Gelatin was also slightly effective. Storage of wine for 10–14 months resulted in a decrease in OA concentration of 22% and 29% for white and red wines, respectively.     

氢化物发生-原子荧光光谱法测定富硒杂粮中的有机硒和无机硒

采用氢化物-原子荧光光谱法与无水乙醇提取相结合的方法测定了富硒杂粮中总硒、无机硒和有机硒的含量,并对仪器的试验参数进行优化。结果表明,富硒杂粮样品中硒主要以有机硒的形态存在,占硒总量的63.02%～95.10%,其中黄玉米有机硒含量最高,达到95.10%。该方法检出限为0.01 μg/L,总硒回收率为97.31%～103.53%,无机硒回收率96.10%～105.45%。本方法操作简单、灵敏度高、回收率好,适合富硒杂粮有机硒和无机硒的测定。     

石墨炉原子吸收法测定富硒酸奶中有机硒

采用超声波破碎,离心、透析的方法将有机硒与无机硒分开,利用微波消解法进行样品消化,减少了消化过程中硒的损失。利用石墨炉球子吸收法对富硒酸奶中有机硒的含量进行测定。用1％Ni（NO3）2作为基体改进剂,灰化温度为900℃,原子化温度为2200℃时,测定甯硒酸奶中有机硒含量,该方法检出限为2．5μg/L,精密度为3．24％～8．27％（RSD）,加标回收率为98．5％～101.3％。该法具有简便、快速、灵敏、稳定、准确等优点,适于富硒酸奶中有机硒的分析测定。     

富硒茶叶中硒的赋存形态研究

利用氢化物—原子荧光光度法分析硒在富硒茶叶中的主要赋存形态及分布规律。结果表明,富硒茶叶中的总硒含量为533.5μg/kg,硒主要以对人体有益的有机结合态形式存在,其含量占总硒的比例为83.66%,而有机硒中最主要的赋存形态为蛋白硒,占有机硒含量的76.35%,茶叶中的硒还有少部分与核酸和多糖结合。     

富硒酵母发酵工艺的优化

以富硒酿酒酵母（Saccharomyces cerevisiae）SY2为发酵菌种,利用5 L发酵罐培养富硒酵母。以富硒酵母生长及硒转化率为评价指标,优化其发酵工艺条件,比较溶氧反馈补料与拟指数补料两种方式对富硒酵母生长、硒转化率等的影响。结果表明,富硒酵母最适发酵条件为：初始pH 5.0,发酵温度30 ℃,接种量8%,硒添加量30 mg/L,发酵时间24 h。在此优化条件下,富硒酵母生物量为9.8 g/L,硒转化率为77.5%。在拟指数补料方式下,培养周期为34 h,富硒酵母得率为0.252 g/g,硒含量为1 920.5 μg/g,硒的转化率为82.7%;在溶氧反馈补料方式下,培养周期为46 h,富硒酵母得率为0.317 g/g,硒含量为1 759.5 μg/g,硒转化率为90.1%。结果显示,拟指数补料培养周期短,生产强度、酵母硒含量较高,是适宜补料方式。     

Evolution of esters in aged Chardonnay wines obtained with different vinification methods

BACKGROUND: During wine ageing on lees yeast lysis takes place and some enzymes from the yeast cells, such as esterases, may be released. These enzymes might determine ester synthesis and could be also involved in their breakdown. In this study, the evolution of esters in Chardonnay wine fermented in stainless steel tanks and aged in bottles (conventional vinification) was compared with the evolution of esters in the same wine fermented and aged in barrel on lees. In this way, it was hoped to determine the influence of distinct methods of vinification on the evolution of esters in Chardonnay wine. RESULTS: The concentration of acetate esters of higher alcohols decreased in all the wines independently of the vinification method. However, the ethyl esters of fatty acids decreased in wine aged in barrel and increased in wine aged in bottle, so it would seem that these compounds interact with the lees present in the barrels and/or with the wood of the barrel. The ethyl esters of organic acids increased during ageing both in barrel and bottle. CONCLUSION: The ageing of Chardonnay wine in barrel on lees did not favour the formation of esters compared to the same wine aged in bottle. Copyright © 2009 Society of Chemical Industry     

The radioecology of the grapevine. 1. The transfer of nuclear weapons fallout from the soil into wine

In a field investigation (1983-1985) comprising eight places of the most important viticultural regions in the Federal Republic of Germany, the contents of the radionuclides tritium (3H), carbon-14 (14C), strontium-90 (90Sr), and cesium-137 (137Cs) in air, soils, leaves of the vine, grapes and wine were measured and site-specific transfer factors were calculated. Data concerning soil parameters, climatic conditions, cultivation and vinification were collected. The tritium content of all samples was 10 Bq/l water of combustion, independent of location and year. The specific activity of 14C in the atmosphere and in biological material was 0.22 Bq/g carbon, independent of site and year. 90Sr contents of soils fluctuated between 0.7 and 3.5 Bq/kg dry matter. The mean content of leaves was 2 Bq/kg fresh material, of grapes 0.035 Bq/kg and of wine 0.008 Bq/l. 137Cs content of soils fluctuated between 1.3 and 7.9 Bq/kg dry matter. The mean content of leaves was 0.098 Bq/kg fresh material, of grapes 0.021 Bq/kg and of wine 0.0085 Bq/l. A relation between transfer of radionuclides and soil parameters and between the contents of grapes and wine was not recognizable. While cultivar-specific differences were not observed in grapes, red wines contained somewhat more 137Cs than white wines. Transfer factors soil grapes were 0.027 for 90Sr and 0.0057 for 137Cs. Site-specific influences such as soil parameters, climate, cultivation, vinification and differences between years led to a relatively small fluctuation of values. An influence of the nuclear power station Neckarwestheim has not been found in any of the radionuclides.     

废弃黄酒糟的开发利用

黄酒糟是黄酒酿造中的主要副产物,黄酒的平均出糟率约为20％～30％,数量相当可观,黄酒糟中残留的蛋白质较多,氨基酸种类齐全,营养价值高,具有广泛开发价值.该文综述了黄酒糟在制备调味品、风味酒、复合氨基酸以及作为酿酒的再生资源等多个领域的应用,为将来黄酒糟的处理以及废弃资源的再生利用提供了参考.     

Speciation of organic and inorganic selenium in selenium-enriched rice by graphite furnace atomic absorption spectrometry after cloud point extraction

A new method was developed for the determination of organic and inorganic selenium in selenium-enriched rice by graphite furnace atomic absorption spectrometry detection after cloud point extraction. Effective separation of organic and inorganic selenium in selenium-enriched rice was achieved by sequentially extracting with water and cyclohexane. Under the optimised conditions, the limit of detection (LOD) was 0.08 μg L⁻¹, the relative standard deviation (RSD) was 2.1% (c = 10.0 μg L⁻¹, n = 11), and the enrichment factor for selenium was 82. Recoveries of inorganic selenium in the selenium-enriched rice samples were between 90.3% and 106.0%. The proposed method was successfully applied for the determination of organic and inorganic selenium as well as total selenium in selenium-enriched rice.