Sombra Lorena L, Luconi Marta O, Fernández Liliana P, Olsina Roberto A, Silva María F, Martínez Luis D
Area de Química Analítica, Facultad de Química, Bioquímica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera (5700), San Luis, Argentina.
J Pharm Biomed Anal. 2003 Jan 1;30(5):1451-8. doi: 10.1016/s0731-7085(02)00483-1.
A micelle-mediated phase separation without added chelating agents to preconcentrate trace levels of aluminium in parenteral solutions as a prior step to its determination by flow injection inductively coupled plasma optical emission spectrometry has been developed. The enrichment step is based on the cloud point extraction of aluminium with the non-ionic surfactant polyethyleneglycolmono-p-nonylphenylether (PONPE 7.5). The chemical variables affecting the sensitivity of the extractive-spectrometric procedure were studied in detail. After optimization, a preconcentration factor of 200 and a %E higher than 99.9 were achieved. The detection limit (DL) value of aluminium for the preconcentration of 50 ml of parenteral solution was 0.25 microgl(-1). The calibration graph using the preconcentration system for aluminium was linear with a correlation coefficient of 0.9997 at levels near the DLs up to at least 200 microgl(-1). The developed hyphenated assay, which thoroughly satisfies the typical requirements for pharmaceutical control processes, is appropriate to monitor the aluminium concentration in parenteral nutrition.
已开发出一种胶束介导的相分离方法,无需添加螯合剂即可对肠外营养液中的痕量铝进行预富集,作为通过流动注射电感耦合等离子体发射光谱法测定铝的前期步骤。富集步骤基于用非离子表面活性剂聚乙二醇单对壬基苯基醚(PONPE 7.5)对铝进行浊点萃取。详细研究了影响萃取光谱法灵敏度的化学变量。优化后,实现了200的预富集因子和高于99.9%的萃取率。对50 ml肠外营养液进行预富集时,铝的检测限(DL)值为0.25 μg l⁻¹。使用铝预富集系统的校准曲线呈线性,在接近检测限的水平下,相关系数为0.9997,至少可达200 μg l⁻¹。所开发的联用分析方法完全满足药物控制过程的典型要求,适用于监测肠外营养中的铝浓度。