MULTIELEMENT ANALYSIS OF MICROSAMPLES OF RENAL FLUIDS

原子光谱学研究的长期目标是发展 并改进了金属和 生物样品中的非金属元素需要微量分析或 痕量分析 分析生物液体微量样品的能力 在现代肾脏生理学中，几种元素是必需的。 技术 这些方法依赖于微量分析， pL至nL范围包括：单个肾单位显微穿刺，分离的 小管微灌注和微注射。 每种分析方法 目前可用的对于某些应用来说有缺点。 也许最 严重的缺陷是，样品，从而分别测定， 通常需要不同的方法。 这一拟议项目的具体目标是： 开发工具和程序， 多元素脉冲空心阴极发射源的评价 分析微观和宏观样品。 主要目标是 用于肾组织所需肾液微量分析的有效方法 research. 第二个目标是确定这种方法的可能效用。 技术作为一般分析跟踪方法;确定是否确实存在 多种金属和非金属可以同时分析，在穆尔- 大小的样品。 亚皮克检测限和良好的精密度已被证明， 该实验室对肾脏主要感兴趣的六种元素中的大多数 使用空心阴极放电的生理学。 除了多元 能力，空心阴极源是唯一能够分析 非金属以及金属在微观和宏观样品。 我们可以 常规地产生具有亚皮克检测限的线性工作曲线 并且我们已经将分析物质量的工作范围扩展到120 pg。接下来， 空心阴极法必须适用于肾样品， 微量元素（K、Ca、Mg和P）在基质中的含量为 许多摩尔的Na和Cl。 此外，少量的 必须评估存在于真实的肾样品中的蛋白质和尿素。 空心阴极放电的脉冲操作将被广泛应用于 研究使用小至0.1 μ s的脉冲宽度，重复率为 高达5KHz，电流高达1A。 铝和石墨阴极将 进行评价，并与铜进行比较，以分析肾功能 流体. 扫描电子显微镜将用于研究微观 对发射信号的精度和强度很重要的影响 从空心阴极来看，这些影响包括：1）电极的侵蚀 表面的溅射和随后的影响，粗糙的表面上 样品激发 2)样品存款的形式或形状， 与样品沉积过程和发射质量相关 信号了

The long range goals of this research in atomic spectroscopy are to develop and improve quantitative methods for the analysis of both metal and nonmetal elements in biological samples requiring either microanalysis or trace analysis. The ability to analyze microsamples of biological fluids for several elements is necessary in modern renal physiology. Techniques which are dependent upon microanalytical and which generate microsamples in the range of pL to nL include: single nephron micropuncture, isolated tubule microperfusion, and microinjection. Each of the analytical methods presently available has drawbacks for some applications. Perhaps the most serious deficiency is that, sample, thus separate determinations by different methods are usually required. The specific goals for this proposed project are to: Develop instrumentation and procedures which will allow objective evaluation of the pulsed hollow cathode emission source for multielement analysis of both micro- and macro samples. The primary objective is a useful method for the microanalysis of renal fluids needed in renal research. A secondary objective is to determine the likely utility of this technique as a general analytical trace method; determine if, indeed, a variety of both metals and nonmetals can be analyzed simultaneously in muL- sized samples. Subpicogram detection limits and good precision have been demonstrated in this laboratory for most of the six elements of prime interest to renal physiology using the hollow cathode discharge. In addition to multielement capability, the hollow cathode source is uniquely capable of analyzing nonmetals as well as metals in both micro- and macrosamples. We can routinely produce linear working curves with subpicogram detection limits and we have extended the working range of analyte mass to 120 pg. Next, the hollow cathode method must be adapted to renal samples in which the minor elements (K, Ca, Mg, and P) are in a matrix of 30 to 150 times as many moles of Na and Cl. In addition, the effect of the small amount of protein and urea present in real renal samples must be evaluated. Pulsed operation of the hollow cathode discharge will be extensively investigated using pulse widths as small as 0.1 mus, repetition rates as high as 5 KHz, and currents up to 1 A. Aluminum and graphite cathodes will be evaluated and compared to that of copper for the analysis of renal fluids. Scanning electron microscopy will be used to study microscopic effects important to the precision and intensity of the emission signal from the hollow cathode, these effects include: 1) Erosion of electrode surfaces by sputtering and subsequent effects of the rough surface on sample excitation. 2) The form or shape of the sample deposit as correlated with sample deposition procedure and the quality of the emission signal.