Departamento de Química Analítica, Universidade Federal Fluminense, Outeiro de São João Batista s/n, Centro, Niterói, RJ 24020-141, Brazil.
J Pharm Biomed Anal. 2013 Feb 23;74:284-90. doi: 10.1016/j.jpba.2012.11.013. Epub 2012 Nov 16.
This paper reports the development of a new method for the focused ultrasound extraction of Cr and Mn from pharmaceutical formulations and their determination by electrothermal atomic absorption spectrometry (ETAAS). The method was optimized by evaluating the influence of several variables such as the sonication power and time, concentration of HCl in the extractant solution and mass of sample employed in the extraction procedure. The curves of pyrolysis and atomization were constructed for both analytes in order to evaluate the effect of the matrix on the measurement of Cr and Mn. Quantitative extraction of both Cr and Mn was achieved when 25-150 mg of the sample were sonicated for 30 min at 50% power with 5 ml of a 1 moll(-1) HCl solution. The developed method was successfully applied in the determination of Cr and Mn in samples of pharmaceutical formulations containing different active principles such as ciprofloxacin, cephalexin, azithromycin, amlodipine and methionine. There was no statistical (95% confidence level, paired t-test) difference between the results obtained by the proposed method and the results obtained after total digestion of the samples.
本文报道了一种从药物制剂中聚焦超声提取 Cr 和 Mn 并用电热原子吸收光谱法(ETAAS)测定的新方法。通过评估超声功率和时间、提取剂溶液中 HCl 浓度以及提取过程中样品质量等几个变量的影响,对该方法进行了优化。为了评估基体对 Cr 和 Mn 测定的影响,分别绘制了两种分析物的热解和原子化曲线。当以 50%的功率对 25-150 mg 样品进行 30 min 超声处理,并使用 5 ml 1 mol/L HCl 溶液作为提取剂时,可实现对 Cr 和 Mn 的定量提取。该方法成功应用于测定含有不同活性成分(如环丙沙星、头孢氨苄、阿奇霉素、氨氯地平和蛋氨酸)的药物制剂中 Cr 和 Mn 的含量。所提出的方法与样品完全消解后得到的结果之间无统计学差异(95%置信水平,配对 t 检验)。