isotope dilution

同位素稀释
  • 文章类型: Journal Article
    数十年来,东亚排放的汞(Hg)增加了中国边海区汞的风险。然而,这些地区汞(尤其是生物可利用汞)的形态尚不清楚。为了解决这个问题,我们分析了黄海(YS)和东海(ECS)的沉积物和孔隙水中的总汞(THg)和甲基汞(MeHg),并使用改进的BCR顺序提取和同位素稀释(ID)技术确定了汞的形态。YS和ECS的近岸区域在沉积物和孔隙水中表现出更高的THg水平,表明陆地投入的重大贡献。甲基汞的空间分布表现出与THg相似的趋势,但是甲基汞浓度较高的位点与THg的位点不一致。改进的BCR顺序提取方法显示,在两个系统中,残留部分占主导地位的汞含量(~44%),具有少量生物可利用的碳酸盐部分(1%)。Spearman相关分析表明,Eh和pH是影响沉积物中汞生物有效性的两个显著因素。汞的生物利用度(BCR法估算)与沉积物中的甲基汞含量呈显著正相关(R²=0.47,P<0.05),表明BCR可用于估计沉积物中汞甲基化的潜力。然而,BCR和ID方法中生物可利用汞的程度分别为1.15±0.38%和29.5±14.8%,分别,这意味着与ID方法相比,BCR技术可能低估了汞的生物利用度(T检验,P<0.01)。
    Mercury (Hg) emitted from East Asian has increased the risk of Hg in China Marginal Seas for decades. However, the speciation of Hg (especially the bioavailable Hg) in these regions remains unclear. To address this problem, we analyzed total Hg (THg) and methylmercury (MeHg) in the sediment and porewater of Yellow sea (YS) and East China Sea (ECS) and determined the speciation of Hg using both improved BCR sequential extraction and isotope dilution (ID) techniques. Nearshore areas of YS and ECS exhibited higher THg levels in sediments and porewater, suggesting the significant contribution of terrestrial inputs. The spatial distribution of MeHg showed similar trends with THg, but the sites with higher MeHg concentrations did not align with those of THg. The improved BCR sequential extraction method showed the residual fraction dominated Hg content (∼44 %) in both systems, with a minor bioavailable carbonate fraction (1 %). The Spearman correlation analysis indicates that Eh and pH are the two factors significantly affected Hg bioavailability in the sediment. The bioavailability of Hg (estimated by the BCR method) showed a significant positive correlation with MeHg levels in the sediment (R²=0.47, P < 0.05), suggesting that BCR can be used to estimate the potential of Hg methylation in the sediment. However, the extent of bioavailable Hg in BCR and ID method were 1.15 ± 0.38 % and 29.5 ± 14.8 %, respectively, implying that Hg bioavailability may be underestimated by BCR techniques compared to ID methods (T-test, P < 0.01).
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  • 文章类型: Journal Article
    背景:液体超负荷与接受透析的儿童的发病率和死亡率相关。准确的临床评估是困难的,使用氧化氘(D2O)测量总体内水(TBW)是不切实际的。我们调查了超声波的使用(美国),生物阻抗谱(BIS),和人体测量学来评估接受维持性血液透析(HD)的儿童的液体清除情况。
    方法:参与者完成了美国,BIS,在HD之前和之后1-2小时进行人体测量,最多可进行五次。美国测量下腔静脉(IVC)直径,肺B线,肌肉弹性成像,和真皮厚度。BIS测量细胞外(ECF)和细胞内(ICF)流体的体积。人体测量包括上臂中部,小腿和脚踝的围,和三头肌皮褶厚度。D2O在HD前进行一次。我们评估了HD前后研究指标的变化,以及研究指标变化与体重变化百分比(%ΔBW)的相关性。我们还评估了通过BIS和D2O测量的TBW之间的一致性。
    结果:招募了8名年龄在3.4-18.5岁的参与者。比较前和后HD测量显示IVC直径显着下降,肺B线,真皮厚度,BIS%ECF,中上臂周长,脚踝,和小腿周长。重复测量相关性显示,BW%与BISECF(rrm=0.51,95%CI0.04,0.80)和小腿周长(rrm=0.80,95%CI0.51,0.92)的变化之间存在显著关系。BISTBW与D2OTBW相关,但高估了TBW2.2升(95%LOA,-4.75至0.42)。
    结论:BIS和小腿围可能有助于评估接受维持性HD的儿童的体液状态变化。IVC直径,肺B线和真皮厚度是未来研究的潜在候选者.
    Fluid overload is associated with morbidity and mortality in children receiving dialysis. Accurate clinical assessment is difficult, and using deuterium oxide (D2O) to measure total body water (TBW) is impractical. We investigated the use of ultrasound (US), bioimpedance spectroscopy (BIS), and anthropometry to assess fluid removal in children receiving maintenance hemodialysis (HD).
    Participants completed US, BIS, and anthropometry immediately before and 1-2 h after HD for up to five sessions. US measured inferior vena cava (IVC) diameter, lung B-lines, muscle elastography, and dermal thickness. BIS measured the volume of extracellular (ECF) and intracellular (ICF) fluid. Anthropometry included mid-upper arm, calf and ankle circumferences, and triceps skinfold thickness. D2O was performed once pre-HD. We assessed the change in study measures pre- versus post-HD, and the correlation of change in study measures with percent change in body weight (%∆BW). We also assessed the agreement between TBW measured by BIS and D2O.
    Eight participants aged 3.4-18.5 years were enrolled. Comparison of pre- and post-HD measures showed significant decrease in IVC diameters, lung B-lines, dermal thickness, BIS %ECF, mid-upper arm circumference, ankle, and calf circumference. Repeated measures correlation showed significant relationships between %∆BW and changes in BIS ECF (rrm =0.51, 95% CI 0.04, 0.80) and calf circumference (rrm=0.80, 95% CI 0.51, 0.92). BIS TBW correlated with D2O TBW but overestimated TBW by 2.2 L (95% LOA, -4.75 to 0.42).
    BIS and calf circumference may be helpful to assess changes in fluid status in children receiving maintenance HD. IVC diameter, lung B-lines and dermal thickness are potential candidates for future studies.
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  • 文章类型: Journal Article
    Mass spectrometry-based methods coupled with stable isotope dilution have become effective and widely used methods for the detection and quantification of food allergens. Current methods target signature peptides resulting from proteolytic digestion of proteins of the allergenic ingredient. The choice of appropriate stable isotope-labelled internal standard is crucial, given the diversity of encountered food matrices which can affect sample preparation and analysis. We propose the use of concatemer, an artificial and stable isotope-labelled protein composed of several concatenated signature peptides as internal standard. With a comparative analysis of three matrices contaminated with four allergens (egg, milk, peanut, and hazelnut), the concatemer approach was found to offer advantages associated with the use of labelled proteins, ideal but unaffordable, and circumvent certain limitations of traditionally used synthetic peptides as internal standards. Although used in the proteomic field for more than a decade, concatemer strategy has not yet been applied for food analysis.
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  • 文章类型: Journal Article
    描述了海水认证参考材料(CRM)NASS-7和CASS-6中痕量金属的认证。在加拿大国家研究委员会(NRC),在测定Cd之前进行柱分离以去除海水基质,Cr,Cu,Fe,Pb,Mn,Mo,Ni,U,V,Zn,而As是在10倍稀释的海水样品中直接测量的,在200倍稀释的海水样品中直接测量B。高分辨率电感耦合等离子体质谱(HR-ICPMS)用于元素分析,用双同位素稀释准确测定B,Cd,Cr,Cu,Fe,Pb,Mo,Ni,U,海水NASS-7和CASS-6中的锌,以及砷的标准添加校准,Co,Mn,V.此外,使用标准添加校准用三重四极杆(QQQ)-ICPMS测量所有分析物,以提供NRC的第二组数据。邀请世界各地的专家实验室为NASS-7和CASS-6中的痕量金属认证提供数据。参与者采用了各种分析方法,包括柱分离,共沉淀,和简单的稀释耦合到ICPMS检测或流动注射分析耦合到化学发光检测,使用双同位素稀释校准,矩阵匹配外部校准,和标准添加校准。这项研究的结果表明,大多数实验室已经证明了其准确测定海水中痕量金属的测量能力。作为这个比较的结果,对海水CRMsNASS-7和CASS-6中的14个元素分配了认证/参考值和相关的不确定度,适用于验证用于海水分析的方法。
    Certification of trace metals in seawater certified reference materials (CRMs) NASS-7 and CASS-6 is described. At the National Research Council Canada (NRC), column separation was performed to remove the seawater matrix prior to the determination of Cd, Cr, Cu, Fe, Pb, Mn, Mo, Ni, U, V, and Zn, whereas As was directly measured in 10-fold diluted seawater samples, and B was directly measured in 200-fold diluted seawater samples. High-resolution inductively coupled plasma mass spectrometry (HR-ICPMS) was used for elemental analyses, with double isotope dilution for the accurate determination of B, Cd, Cr, Cu, Fe, Pb, Mo, Ni, U, and Zn in seawater NASS-7 and CASS-6, and standard addition calibration for As, Co, Mn, and V. In addition, all analytes were measured using standard addition calibration with triple quadrupole (QQQ)-ICPMS to provide a second set of data at NRC. Expert laboratories worldwide were invited to contribute data to the certification of trace metals in NASS-7 and CASS-6. Various analytical methods were employed by participants including column separation, co-precipitation, and simple dilution coupled to ICPMS detection or flow injection analysis coupled to chemiluminescence detection, with use of double isotope dilution calibration, matrix matching external calibration, and standard addition calibration. Results presented in this study show that majority of laboratories have demonstrated their measurement capabilities for the accurate determination of trace metals in seawater. As a result of this comparison, certified/reference values and associated uncertainties were assigned for 14 elements in seawater CRMs NASS-7 and CASS-6, suitable for the validation of methods used for seawater analysis.
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  • 文章类型: Journal Article
    An accurate, rapid and effective method was established for determination of eugenol in plasma, muscle, skin, liver, kidney and gill of fish using gas chromatography-ion trap tandem mass spectrometry. Samples of muscle, skin, liver, kidney and gill were prepared using the modified QuEChERS (quick, easy, cheap, effective, rugged and safe) procedure, and a plasma sample was prepared by a liquid-liquid extraction procedure. Eugenol was monitored in <7 min using an electron-ionization source in MS/MS mode and quantified by an internal standard of eugenol-d3 . The limit of detection was 5.0 μg/kg, and the limit of quantification was 10.0 μg/kg. The calibration curve was linear in the range of 5-1000 μg/L (R2 = 0.9996). Intra- and inter-day precisions of eugenol expressed as relative standard deviation were within 9.74%, and the accuracy exhibited a relative error ranging from -2.20 to 8.89%. The developed method was successfully used to study the elimination regularity of eugenol in mandarin fish.
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  • 文章类型: Comparative Study
    The total haemoglobin (Hb) concentration in blood is one of the most frequently measured analytes in clinical medicine because of its significance for evaluating the health state of a human. The spectrophotometric cyanmethaemoglobin (HiCN) method is the internationally accepted conventional reference method to determine this biomarker. It is frequently used in clinical routine diagnostics but is not traceable to the International System of Units and thus does not meet highest metrological demands. A further critical issue is the toxicity of the necessary potassium cyanide. Different methods to solve these problems are reported here. They all were validated against the HiCN method in an interlaboratory comparison by measuring the total Hb concentration present in the certified reference material JCCRM 912-2M. Methods considered were the spectrophotometric alkaline haematin detergent (AHD) method as well as several isotope dilution (ID)-based approaches. The latter include inductively coupled plasma mass spectrometry (ICP-MS), species-specific (SS) ICP-MS, organic MS and Raman spectrometry. Graphical abstract ᅟ.
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