In public health studies limited volumes of blood are often collected and stored for future hypothesis testing. Archived samples are irreplaceable and therefore it is valuable to develop analytical techniques that req...In public health studies limited volumes of blood are often collected and stored for future hypothesis testing. Archived samples are irreplaceable and therefore it is valuable to develop analytical techniques that require minimal sample vo-lume. This work describes the measurement of trace elements Mg, Cu, Fe, Zn and ultratrace elements Cd, Co, Mn, Pb in limited quantity (150 μL) human serum or plasma samples. Samples were digested using a hotblock and analyzed using inductively coupled plasma mass spectrometry (ICP-MS). The analytical method was evaluated using a quadrupole (Q) and sector field high resolution (SF) instrument to analyze trace elements in Seronorm? quality control serum material. The method was used to analyze 1888 blinded human plasma samples which were archived for the National Cancer Institute from the Nutrition Intervention Trial in Linxian China. The inductively coupled plasma method was capable of accurately analyzed limited quantity samples of human serum and plasma for the trace elements Mg, Cu, Fe Zn and the ultra trace elements Co, Mn and Pb. The concentration of Cd in human plasma samples was below the level of detection for 75% of the samples analyzed.展开更多
研究建立了四级杆碰撞反应池-ICP-MS法(Inductively coupled plasma mass spectrometry,ICP-MS)测定维生素及其预混料中铅、总砷和总汞的检测方法。样品加入硝酸,经微波消解后定容至100 m L,待测液采用四级杆碰撞反应池-ICP-MS法进行测...研究建立了四级杆碰撞反应池-ICP-MS法(Inductively coupled plasma mass spectrometry,ICP-MS)测定维生素及其预混料中铅、总砷和总汞的检测方法。样品加入硝酸,经微波消解后定容至100 m L,待测液采用四级杆碰撞反应池-ICP-MS法进行测定。由于汞易挥发,实验中优化了消解的温度。维生素B_(12)样品中存在钴元素的干扰,以^(75)砷(As)和内标元素^(73)锗(Ge)的信号强度比值与砷元素的浓度成正比,采用碰撞反应池技术、氦气动能歧视(Kinetic energy discrimination,KED)模式进行定量分析,计算结果为样品中As和Co-O结合物的总含量;再以^(59)钴(Co)和内标元素^(45)钪(Sc)的信号强度比值与钴元素的浓度成正比,采用同样方法进行定量分析,得出钴的含量。最后通过计算两者之差得出样品中砷的含量。试验结果表明:铅、总砷和钴在1.0~50.0μg/L范围内线性关系良好,相关系数R均大于0.999。在不同加标水平下,3种元素的回收率范围在88.3%~104.3%之间,汞在0.1~2.0μg/L范围内线性关系良好,相关系数R为0.998。在不同加标水平下,汞元素的回收率范围在88.3%~104.3%之间,相对标准偏差(RSD)均小于10%。该方法操作简便、快速准确,适用于维生素及其预混料中铅、总砷、总汞元素的同时检测。展开更多
文摘In public health studies limited volumes of blood are often collected and stored for future hypothesis testing. Archived samples are irreplaceable and therefore it is valuable to develop analytical techniques that require minimal sample vo-lume. This work describes the measurement of trace elements Mg, Cu, Fe, Zn and ultratrace elements Cd, Co, Mn, Pb in limited quantity (150 μL) human serum or plasma samples. Samples were digested using a hotblock and analyzed using inductively coupled plasma mass spectrometry (ICP-MS). The analytical method was evaluated using a quadrupole (Q) and sector field high resolution (SF) instrument to analyze trace elements in Seronorm? quality control serum material. The method was used to analyze 1888 blinded human plasma samples which were archived for the National Cancer Institute from the Nutrition Intervention Trial in Linxian China. The inductively coupled plasma method was capable of accurately analyzed limited quantity samples of human serum and plasma for the trace elements Mg, Cu, Fe Zn and the ultra trace elements Co, Mn and Pb. The concentration of Cd in human plasma samples was below the level of detection for 75% of the samples analyzed.
文摘研究建立了四级杆碰撞反应池-ICP-MS法(Inductively coupled plasma mass spectrometry,ICP-MS)测定维生素及其预混料中铅、总砷和总汞的检测方法。样品加入硝酸,经微波消解后定容至100 m L,待测液采用四级杆碰撞反应池-ICP-MS法进行测定。由于汞易挥发,实验中优化了消解的温度。维生素B_(12)样品中存在钴元素的干扰,以^(75)砷(As)和内标元素^(73)锗(Ge)的信号强度比值与砷元素的浓度成正比,采用碰撞反应池技术、氦气动能歧视(Kinetic energy discrimination,KED)模式进行定量分析,计算结果为样品中As和Co-O结合物的总含量;再以^(59)钴(Co)和内标元素^(45)钪(Sc)的信号强度比值与钴元素的浓度成正比,采用同样方法进行定量分析,得出钴的含量。最后通过计算两者之差得出样品中砷的含量。试验结果表明:铅、总砷和钴在1.0~50.0μg/L范围内线性关系良好,相关系数R均大于0.999。在不同加标水平下,3种元素的回收率范围在88.3%~104.3%之间,汞在0.1~2.0μg/L范围内线性关系良好,相关系数R为0.998。在不同加标水平下,汞元素的回收率范围在88.3%~104.3%之间,相对标准偏差(RSD)均小于10%。该方法操作简便、快速准确,适用于维生素及其预混料中铅、总砷、总汞元素的同时检测。