Abstract

Here is reported the development of methods for the determination of Al, Cd, Cu, Mo, and Pb by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR–CS GFAAS) after microwave-assisted acid digestion in pharmaceuticals for patients with chronic kidney disease. The measurements were performed at the primary lines of the analytes. The optimum pyrolysis and atomization temperatures were 1800 and 2700 °C for Al, 600 and 1600 °C for Cd, 1400 and 2200 °C for Cu, 1400 and 2600 °C for Mo and 900, and 2400 °C for Pb, respectively. Palladium was used as a chemical modifier for Pb, while Mg(NO₃)₂ was employed for Al, Cd, and Cu. The validation parameters (linearity, analytical range, accuracy, precision, limit of quantification, and specificity) were obtained according to the stipulations in the Chapter American Pharmacopeia <233>. The limit of detection was 1.63 μg L⁻¹ for Al, 0.02 μg L⁻¹ for Cd, 0.49 μg L⁻¹ for Cu, 0.76 μg L⁻¹ for Mo, and 0.59 μg L⁻¹ for Pb. The precision was between 2.1% for Mo and 8.1% for Al. The recoveries were from 90.2% for Pb to 106.1% for Cd. The developed methods were successfully applied to determine the five analytes in 50 pharmaceutical formulations. Cadmium, Cu, and Mo concentrations were within the maximum limits recommended by the Brazilian Pharmacopeia in all medicines. However, six drug products had a Pb concentration higher than the limit for this element. All samples analyzed showed relatively high concentrations of Al.

摘要

本文报道了慢性病患者药物中微波辅助酸消解后高分辨连续源石墨炉原子吸收光谱法 (HR-CS GFAAS) 测定 Al、Cd、Cu、Mo 和 Pb 方法的进展。肾脏疾病。测量在分析物的主要线进行。最佳热解和雾化温度分别为 Al 1800 和 2700 ℃，Cd 600 和 1600 ℃，Cu 1400 和 2200 ℃，Mo 和 900 1400 和 2600 ℃，Pb 分别为 2400 ℃。钯用作 Pb 的化学改性剂，而 Mg(NO ₃ ) ₂用于 Al、Cd 和 Cu。验证参数（线性、分析范围、准确度、精密度、定量限、特异性）均按照美国药典<233>章节的规定获得。检测限为 Al 1.63 μg L ^-1、Cd 0.02 μg L ^{-1 、Cu 0.49 μg L -1} 、Mo 0.76 μg L ^-1和0.59 μg L ^-1对于铅。Mo 的精度在 2.1% 和 Al 的 8.1% 之间。回收率从 Pb 的 90.2% 到 Cd 的 106.1%。所开发的方法成功地应用于测定 50 种药物制剂中的五种分析物。镉、铜和钼的浓度均在巴西药典推荐的所有药物的最大限量范围内。然而，六种药品的铅浓度高于该元素的限值。分析的所有样品都显示出相对高浓度的铝。