Background: In the context of a nuclear reactor accident, thyroid is the main target organ of radioactive iodines. To avoid as much as possible thyroid disorders or even cancer development, it is recommended to admini...Background: In the context of a nuclear reactor accident, thyroid is the main target organ of radioactive iodines. To avoid as much as possible thyroid disorders or even cancer development, it is recommended to administer a single dose of potassium iodide to people at risk of exposure. Nevertheless, the Fukushima Dai-ichi disaster has pointed out many questions about the conditions of stable iodine prophylaxis implementation highlighting the need for reflection further revision of the actual “iodine doctrine”. Therefore, providing useful data is required notably through the implementation of animal experiments to strengthen current knowledge and to edit new recommendations. Methods: Urinary iodine constitutes a very good indicator to investigate the function of thyroid, its interpretation demands reliable analyses. Prior to perform animal experiments, two calibration methods were designed by our lab and compared together (standard addition and external calibration) to assess the urinary concentration of stable iodine in urine by ICP-MS. They were validated based on several key parameters especially linearity, accuracy and limits of detection (LOD) and quantification (LOQ). Results: The results were nicely satisfying. Indeed, both calibration methods have indicated very good coefficients of correlations, accuracies with low expanded relative uncertainties were obtained. The estimated LOD in the sample for standard addition method and external calibration were fully acceptable, 0.39 μg·L-1 and 0.35 μg·L-1, respectively. All performance criteria have been thus fulfilled successfully. The established methods were proven to be accurate, robust and sensitive. Once validated, both calibration methods were applied to rat urine samples and the results of z-score and Wilcoxon W test concluded that there were no statistically significant differences between both methods.展开更多
在解析特殊挥发性物质的质谱裂解行为的基础上,建立气相色谱-质谱联用单离子监测(gas chromatography-mass spectrometry with selected ion monitoring,GC-MS SIM)稳定同位素内标法,对不同品种葡萄果实中的58种挥发性物质进行精准的定...在解析特殊挥发性物质的质谱裂解行为的基础上,建立气相色谱-质谱联用单离子监测(gas chromatography-mass spectrometry with selected ion monitoring,GC-MS SIM)稳定同位素内标法,对不同品种葡萄果实中的58种挥发性物质进行精准的定性与定量分析,并探讨不同品种中挥发性物质的含量差异。葡萄果实样品破碎均质后,采用固相微萃取的方法进行高效富集萃取,再进行GC-MS SIM分析。结果表明,在特定的质量浓度范围内该方法线性关系良好,其线性相关系数在0.995 0(除异丙醇为0.967 1)以上;绝大多数目标物的检出限低于1.56μg/kg;除个别挥发性物质的加标回收率较低,不同加标水平目标物样品回收率在60.64%~129.63%范围内,其回收率结果的相对标准偏差均低于19.56%。该方法具有灵敏度高、准确可靠的优点,适用于葡萄等水果蔬菜中挥发性物质的准确定性与定量研究。此外,本实验通过对12个不同品种的葡萄果实样品中挥发性物质的差异分析,探明葡萄果实中的关键性挥发性物质,并挖掘出不同品种葡萄的特色挥发性物质。展开更多
A new method for high-precision measurements of stable (δ88/86Sr) and radiogenic (87Sr/86Sr) Sr isotope ratios was developed on the MC-ICP-MS using a standard-sample-standard bracketing protocol. By carefully monitor...A new method for high-precision measurements of stable (δ88/86Sr) and radiogenic (87Sr/86Sr) Sr isotope ratios was developed on the MC-ICP-MS using a standard-sample-standard bracketing protocol. By carefully monitoring and controlling the accumulation of the on-peak backgrounds (i.e. the carryover memory) on the instrument, our method can provide an external precision of around 0.010‰ to 0.014‰ for 88/86 Sr measurements. Such precision is comparable to that achieved by double-spike TIMS method (DS-TIMS), and 2-3 times better than those of the previously reported results by MC-ICP-MS without spiking. The results of the standard seawater IAPSO are also identical to those by DS-TIMS. However, our method is more advantageous, efficient and convenient to use for routine Sr isotopic analysis than the DS-TIMS method as there is no need to prepare and calibrate the 84Sr-87 Sr double spike. Using this method, we measured the δ88/86Sr values in a series of international geological rock standards, which show large variability, with the lowest value (0.20‰) registered in JG-2, a terrestrial granite, and the highest value (0.539‰) in UB-N, a serpentinite. This may provide an additional means for isotopic characterization of geological processes, adding a new dimension over the traditional use of radiogenic Sr isotopic ratio 87Sr/86Sr.展开更多
测量环境及仪器间光谱信号的差异导致近红外光谱模型从主机传递到从机后,经常会产生过大误差。本研究提出了一种基于稳定一致波长筛选的无标样近红外模型传递方法(Screening stable and consistent wavelengths,SSCW),剔除主从仪器间差...测量环境及仪器间光谱信号的差异导致近红外光谱模型从主机传递到从机后,经常会产生过大误差。本研究提出了一种基于稳定一致波长筛选的无标样近红外模型传递方法(Screening stable and consistent wavelengths,SSCW),剔除主从仪器间差谱的标准偏差大于样品精密度测试光谱标准偏差的波长,以及精密度测试偏差过大的波长,筛选出仪器间光谱信号一致性好且稳定的波长建立近红外光谱定标模型。分别以玉米和黄芩样本集对本算法的有效性进行了检验。结果表明,SSCW模型传递后对从机样品的预测均方根残差RMSEP较全波长PLS模型直接传递结果小一个量级,大部分情况下优于分段直接校正算法(Piecewise direct standardization,PDS)的结果和文献报道的无标样模型传递结果。本方法具有传递性能好、模型参数少、稳健等优点,在不同仪器间可实现近红外光谱模型的无标样传递。展开更多
基金partly supported by the French National“Investment for the future”funding programme.
文摘Background: In the context of a nuclear reactor accident, thyroid is the main target organ of radioactive iodines. To avoid as much as possible thyroid disorders or even cancer development, it is recommended to administer a single dose of potassium iodide to people at risk of exposure. Nevertheless, the Fukushima Dai-ichi disaster has pointed out many questions about the conditions of stable iodine prophylaxis implementation highlighting the need for reflection further revision of the actual “iodine doctrine”. Therefore, providing useful data is required notably through the implementation of animal experiments to strengthen current knowledge and to edit new recommendations. Methods: Urinary iodine constitutes a very good indicator to investigate the function of thyroid, its interpretation demands reliable analyses. Prior to perform animal experiments, two calibration methods were designed by our lab and compared together (standard addition and external calibration) to assess the urinary concentration of stable iodine in urine by ICP-MS. They were validated based on several key parameters especially linearity, accuracy and limits of detection (LOD) and quantification (LOQ). Results: The results were nicely satisfying. Indeed, both calibration methods have indicated very good coefficients of correlations, accuracies with low expanded relative uncertainties were obtained. The estimated LOD in the sample for standard addition method and external calibration were fully acceptable, 0.39 μg·L-1 and 0.35 μg·L-1, respectively. All performance criteria have been thus fulfilled successfully. The established methods were proven to be accurate, robust and sensitive. Once validated, both calibration methods were applied to rat urine samples and the results of z-score and Wilcoxon W test concluded that there were no statistically significant differences between both methods.
基金supported by the Chinese Ministry of Science and Technology Special Scheme (2009CB421206 and 2010CB808900)the Knowledge Innovation Program of the Chinese Academy of Sciences (KZCX2-YW-138)+1 种基金the National Natural Science Foundation of China (40973008 and 41173006)contribution No.IS-1616 from GIGCAS
文摘A new method for high-precision measurements of stable (δ88/86Sr) and radiogenic (87Sr/86Sr) Sr isotope ratios was developed on the MC-ICP-MS using a standard-sample-standard bracketing protocol. By carefully monitoring and controlling the accumulation of the on-peak backgrounds (i.e. the carryover memory) on the instrument, our method can provide an external precision of around 0.010‰ to 0.014‰ for 88/86 Sr measurements. Such precision is comparable to that achieved by double-spike TIMS method (DS-TIMS), and 2-3 times better than those of the previously reported results by MC-ICP-MS without spiking. The results of the standard seawater IAPSO are also identical to those by DS-TIMS. However, our method is more advantageous, efficient and convenient to use for routine Sr isotopic analysis than the DS-TIMS method as there is no need to prepare and calibrate the 84Sr-87 Sr double spike. Using this method, we measured the δ88/86Sr values in a series of international geological rock standards, which show large variability, with the lowest value (0.20‰) registered in JG-2, a terrestrial granite, and the highest value (0.539‰) in UB-N, a serpentinite. This may provide an additional means for isotopic characterization of geological processes, adding a new dimension over the traditional use of radiogenic Sr isotopic ratio 87Sr/86Sr.
文摘测量环境及仪器间光谱信号的差异导致近红外光谱模型从主机传递到从机后,经常会产生过大误差。本研究提出了一种基于稳定一致波长筛选的无标样近红外模型传递方法(Screening stable and consistent wavelengths,SSCW),剔除主从仪器间差谱的标准偏差大于样品精密度测试光谱标准偏差的波长,以及精密度测试偏差过大的波长,筛选出仪器间光谱信号一致性好且稳定的波长建立近红外光谱定标模型。分别以玉米和黄芩样本集对本算法的有效性进行了检验。结果表明,SSCW模型传递后对从机样品的预测均方根残差RMSEP较全波长PLS模型直接传递结果小一个量级,大部分情况下优于分段直接校正算法(Piecewise direct standardization,PDS)的结果和文献报道的无标样模型传递结果。本方法具有传递性能好、模型参数少、稳健等优点,在不同仪器间可实现近红外光谱模型的无标样传递。
