流动注射-火焰原子吸收光谱法在线预富集测定注射剂中的铬

On-line preconcentration and determination of chromium in parenteral solutions by flow injection-flame atomic absorption spectrometry.

作者信息

Wuilloud Gustavo M, Wuilloud Rodolfo G, de Wuilloud Jorgelina C A, Olsina Roberto A, Martinez Luis D

机构信息

Area de Química Analítica, Facultad de Química, Bioquímica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera, PO Box 375, 5700 San Luis, Argentina.

出版信息

J Pharm Biomed Anal. 2003 Feb 5;31(1):117-24. doi: 10.1016/s0731-7085(02)00604-0.

DOI:10.1016/s0731-7085(02)00604-0

PMID:12560055

Abstract

An on-line chromium preconcentration and determination system implemented with flame atomic absorption spectrometry (FAAS) associated to flow injection (FI) was studied. For the retention of chromium, 4-(2-Thiazolylazo)-resorcinol (TAR) and Amberlite XAD-16 were used, at pH 5.0. The Cr-TAR complex was removed from the micro-column with ethanol. An enrichment factor of 50 was obtained for the preconcentration of 50 ml of sample solution. The detection limit value for the preconcentration of 50 ml of aqueous solution of Cr was 20 ng l(-1). The precision for ten replicate determinations at the 5 microg l(-1) Cr levels was 2.9% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for chromium was linear with a correlation coefficient of 0.9997 at levels near the detection limits up to at least 100 microg l(-1). The method was successfully applied to the determination of chromium in parenteral solution samples.

摘要

研究了一种采用火焰原子吸收光谱法（FAAS）与流动注射（FI）联用的在线铬预富集和测定系统。为保留铬，在pH 5.0条件下，使用4-（2-噻唑基偶氮）间苯二酚（TAR）和Amberlite XAD-16。用乙醇从微柱中洗脱Cr-TAR络合物。对50 ml样品溶液进行预富集时，富集因子为50。对50 ml铬水溶液进行预富集时的检测限为20 ng l(-1)。在5 μg l(-1)铬水平下进行十次重复测定的精密度为相对标准偏差（RSD）2.9%（根据所得峰高计算）。使用铬预富集系统得到的校准曲线在接近检测限至至少100 μg l(-1)的水平范围内呈线性，相关系数为0.9997。该方法成功应用于肠胃外溶液样品中铬的测定。