Huffer J W, Westcott J E, Miller L V, Krebs N F
Department of Pediatrics, University of Colorado Health Sciences Center, Denver 80262, USA.
Anal Chem. 1998 Jun 1;70(11):2218-20. doi: 10.1021/ac971083d.
A microwave digestion method to prepare human erythrocytes for measurement of Zn concentration by atomic absorption spectrophotometry and stable isotope enrichment by mass spectrometry is described. Also described is a process for purifying digested erythrocyte samples enriched with Zn stable isotope for analysis by fast atom bombardment mass spectrometry. Microwave digestion was investigated as a way to increase sample throughput by replacing a more time-consuming conventional oven ashing/hot plate wet digestion method. Pooled red blood cells and NIST bovine liver standard reference material were digested by the two different methods and zinc recoveries compared by atomic absorption spectrophotometry. Microwave and conventional methods yielded 11.7 +/- 0.1 and 11.7 +/- 0.2 micrograms/g (wet wt), respectively, for the pooled erythrocytes, and Zn recovery from NIST bovine liver standard (certified 123 +/- 8 micrograms/g) was 128.2 +/- 1.2 and 127.4 +/- 1.3 micrograms/g, p > or = 0.282, respectively. Microwave digestion improved the processing of erythrocytes for atomic absorption spectrophotometry and mass spectrometry by reducing digestion time from 1 week to 2 h. In addition, a procedure for purifying digested erythrocyte samples by either extraction and ion-exchange chromatography in preparation for mass spectrometry analysis of Zn stable isotope enrichment is outlined.
本文描述了一种微波消解方法，用于制备人红细胞，以便通过原子吸收分光光度法测定锌浓度，并通过质谱法进行稳定同位素富集。还描述了一种纯化富含锌稳定同位素的消化红细胞样品的方法，用于通过快原子轰击质谱法进行分析。研究了微波消解作为一种增加样品通量的方法，以取代耗时更长的传统炉内灰化/热板湿法消解方法。用这两种不同方法对混合红细胞和NIST牛肝标准参考物质进行消解，并通过原子吸收分光光度法比较锌的回收率。对于混合红细胞，微波法和传统方法分别得到11.7±0.1和11.7±0.2微克/克（湿重），从NIST牛肝标准物质（认证值为123±8微克/克）中回收的锌分别为128.2±1.2和127.4±1.3微克/克，p≥0.282。微波消解通过将消解时间从1周缩短至2小时，改善了用于原子吸收分光光度法和质谱法的红细胞处理过程。此外，概述了一种通过萃取和离子交换色谱法纯化消化红细胞样品的程序，以准备对锌稳定同位素富集进行质谱分析。
