Georgiades C A
Warner-Lambert Co., Consumer Products Research and Development, Morris Plains, NJ 07950.
J Assoc Off Anal Chem. 1990 May-Jun;73(3):385-8.
A sensitive, specific, automated energy dispersive X-ray fluorescence (EDXRF) method for determination of anhydrous dihydroxyaluminum sodium carbonate in antacid tablets has been developed. The compound was quantitated by impact grinding, pelletizing at 10 tons pressure, and monitoring the aluminum by using a rhodium anode X-ray tube, high resolution thermoelectrically cooled Si(Li) detector with sample spinning, and computer data processing. The assay procedure was validated with spiked laboratory-prepared samples at 100 +/- 20% levels. The average recovery was 100.6% with a relative standard deviation of 1.6% (n = 14). Instrument precision was determined and found to have an average relative standard deviation of 1.0% (n = 16). In addition, analysis precision by the EDXRF method was compared to that for titration and autoanalyzer methodologies and found to be statistically comparable. The sample precision had an averaged relative standard deviation of 2.7% (n = 16) by X-ray methodology. The advantages of this EDXRF method include increased sample throughout with excellent precision and accuracy, no solvent usage, and automated data handling.
已开发出一种灵敏、特异的自动化能量色散X射线荧光（EDXRF）方法，用于测定抗酸片中的无水二羟基铝碳酸钠。通过冲击研磨、在10吨压力下压片，并使用铑阳极X射线管、带样品旋转的高分辨率热电冷却硅（锂）探测器以及计算机数据处理来对该化合物进行定量。用加标实验室制备的样品在100±20%水平验证了测定程序。平均回收率为100.6%，相对标准偏差为1.6%（n = 14）。测定了仪器精密度，发现平均相对标准偏差为1.0%（n = 16）。此外，将EDXRF方法的分析精密度与滴定法和自动分析仪方法的精密度进行了比较，发现具有统计学可比性。通过X射线方法，样品精密度的平均相对标准偏差为2.7%（n = 16）。这种EDXRF方法的优点包括提高了样品通量，具有出色的精密度和准确度，无需使用溶剂，以及自动化数据处理。
