Development of a routine analysis of 4-mercapto-4-methylpentan-2-one in wine by stable isotope dilution assay and mass tandem spectrometry

The 4-mercapto-4-methylpentan-2-one (4MMP) is a key aroma compound in wines, especially in Sauvignon Blanc ones. Its accurate quantification is quite difficult due to its traces levels and its reactivity in wine conferred by the thiol function. In this paper, we proposed a new method for its quantification in wine without any sample preparation, based on automated derivatization procedure by methoximation and SIDA–SPME–GC–MS/MS analysis. The derivatization procedure was adapted from a previously published method in order to decrease the amount of reagents and the volume of wine (only 3 mL are required). The use of SPME and the detection conditions have also been optimized to reach the best sensitivity as possible. The method was then validated according to the International Organization of Vine and Wine recommendations and exhibited excellent performances. Indeed, this method allowed us to quantify the 4MMP in wine at traces levels (LOD = 0.19 ng L⁻¹) with reproducible results (RSD < 15%) and a very good accuracy (recovery = 102%).     

Broadband WET: a novel technique for quantitative characterization of minor components in foods

NMR analysis of foods frequently suffers from a problem of dynamic range, which limits the detection of minor components due to the huge signals of water and major components such as sugars. In the present study, we propose a new method named as ‘broadband WET’. This pulse scheme was applied to persimmon fruit juice for saturating the resonances of water and sugars, which covered a broad bandwidth. In comparison with the conventional solvent suppression methods such as WET and DPFGSE‐WATERGATE, it was shown that broadband WET provided highly selective suppression of resonances covering an extensive bandwidth and quantitative signals of minor components without distortion. The proposed method is suitable to detect quantitative signals of the minor components with a high sensitivity. Copyright © 2014 John Wiley & Sons, Ltd.     

A sensitive and selective method for the quantitative analysis of miglitol in rat plasma using unique solid‐phase extraction coupled with liquid chromatography–tandem mass spectrometry

A sensitive, selective and robust liquid chromatography–tandem mass spectrometry (LC‐MS/MS) method was developed for the quantification of miglitol in rat plasma. The sample preparation procedures involved protein precipitation and unique solid‐phase extraction, which efficiently removed sources of ion suppression and column degradation interference present in the plasma. Chromatographic separation was achieved on an amide column using 10 mmol/L CH₃COONH₄ and CH₃CN:CH₃OH (90:10, v/v) as the mobile phase under gradient conditions. Detection was performed using tandem mass spectrometry equipped with an electrospray ionization interface in positive ion mode.The selected reaction monitoring transitions for miglitol and a stable isotope‐labeled internal standard were m/z 208 → m/z 146 and m/z 212 → m/z 176, respectively. The correlation coefficients of the calibration curves ranged from 0.9984 to 0.9993 over a concentration range of 0.5–100 ng/mL plasma. The quantification limit of the proposed method was more than 10 times lower than those of previously reported LC‐MS/MS methods. The novel method was successfully validated and applied to a pharmacokinetic study in rats. Copyright © 2014 John Wiley & Sons, Ltd.     

两种测量透镜焦距方法实验结果的不确定度评定

介绍了等精度和不等精度两种测量透镜焦距的方法及相应实验数据的处理，并对两种方法进行了比较。     

Schwarzschild-de-Sitter黑洞宇宙视界量子态的熵

采用由广义不确定关系得到的新的态密度方程，研究了Schwarzchild-de-Sitter时空背景下黑洞宇宙视界的熵.利用新的态密度方程，克服了用brick wall模型方法计算黑洞熵，在消除紫外发散需取截断的不完善之处，以此揭示了黑洞熵与其视界面积成正比这一内在联系，进一步表明黑洞熵是视界面处量子态的熵. 关键词： 黑洞 广义不确定关系 态密度 熵     

Schwarzschild-de Sitter黑洞宇宙视界量子态的熵

采用由广义不确定关系得到的新的态密度方程 ,研究了Schwarzchild deSitter时空背景下黑洞宇宙视界的熵 .利用新的态密度方程 ,克服了用brick wall模型方法计算黑洞熵 ,在消除紫外发散需取截断的不完善之处 ,以此揭示了黑洞熵与其视界面积成正比这一内在联系 ,进一步表明黑洞熵是视界面处量子态的熵     

The traceability of analytical measurements

 Traceability to the System International (SI) is an important prerequisite for international comparability and uniformity of chemical measurements to ensure mutual recognition of the results. In theory, all measurements can be traced back to the seven base units of the SI. Although the traceability system works well for most physical measurements, in many analytical and in some spectrophotometric measurements this system is not satisfactory. This paper describes the particular and practical problems and the contribution of the Romanian National Institute of Metrology in this field. The paper discusses the following concepts: clearly defined targets in the form of requirement specification, knowledge of trueness and/or measurement uncertainty, and traceability through an unbroken chain of calibration to primary standards. Traceability and uncertainty being two concepts inherently coupled, two examples of assessment of the uncertainty of measurement results are given for two spectrophotometric methods currently used in chemical laboratories. Received: 17 July 1996 Accepted: 2 September 1996     

有效数字概念的局限性

通过分析按有效数字定义近似处理标准误差前后引起包含测量结果真值概率的变化，指出现行有效数字概念有一定的局限性，明确了为克服这个局限性，不确定度有时应采取两位数表示。     

MISSED OPPORTUNITIES IN NATURAL RESOURCE MANAGEMENT

After 20 years of effort, technical approaches to natural resource management have not been effective in preventing overuse and destruction of resources. The resource modeling community can help to change our present course toward destruction by (1) recognizing and publicizing the ineffectiveness of scientific, technical and magical approaches to resource management, (2) pointing out that the resolution of environmental problems is impossible unless the social problems of excessive human population sizes and excessive consumption are effectively addressed, (3) making clear the irrationality and imprudence of current environmental decisionmaking under uncertainty, and (4) pointing out the impossibility of achieving conservation goals by management that attempts to achieve economic optima.     

Haar-Gaussian小波变换在边缘测量中的应用

应用Harr-Gaussian小波变换对图形图像的边缘进行频域分析，建立边缘测量的物理模型， 并用带宽匹配方法和远心测量光学系统，在大景深物体测量中获得准确的结果. 关键词： 小波变换 边缘测量 测不准原理 远心系统 图像识别 自动检测