Baranda Ana B, Jiménez Rosa M, Alonso Rosa M
Departamento de Química Analítica, Facultad de Ciencias, Universidad del País Vasco/EHU, Apdo. 644, 48080 Bilbao, Spain.
J Chromatogr A. 2004 Mar 26;1031(1-2):275-80. doi: 10.1016/j.chroma.2003.11.019.
A high-performance liquid chromatographic method with electrochemical detection was developed for the simultaneous determination of five 1,4-dihydropyridines: amlodipine, nitrendipine, felodipine, lacidipine and lercanidipine. These drugs are widely used in the treatment of hypertension, angina pectoris and the therapy of cerebrovascular spasms of various origins. The chromatographic separation was performed on a Supelcosil LC ABZ + Plus C18 column with a mobile phase consisting of acetonitrile-10 mM acetate buffer (72:28, v/v) at a flow rate of 1 ml/min. The temperature was set at 30 +/- 0.2 degrees C. The amperometric detector, equipped with a glassy carbon electrode was operated at +1100 mV versus Ag/AgCl in the direct current mode. Under these chromatographic conditions, the drugs eluted in less than 12 min. The method showed to be linear over the range 4.5-15 microg/ml with a within-day and day-to-day repeatabilities in terms of R.S.D. lower than 15%, an accuracy greater than 98% and detection limits varying from 90 ng/ml (amlodipine) to 1.55 microg/ml (nitrendipine). The method was successfully applied to commercially available pharmaceuticals with relative errors lower than 5%. The validity of the method was examined comparing the results obtained with those of HPLC with photometric detection.
建立了一种带电化学检测的高效液相色谱法，用于同时测定5种1,4 - 二氢吡啶类药物：氨氯地平、尼群地平、非洛地平、拉西地平和乐卡地平。这些药物广泛用于治疗高血压、心绞痛以及各种原因引起的脑血管痉挛。色谱分离在Supelcosil LC ABZ + Plus C18柱上进行，流动相由乙腈 - 10 mM乙酸盐缓冲液（72:28，v/v）组成，流速为1 ml/min。温度设定为30±0.2℃。配备玻碳电极的安培检测器在直流模式下相对于Ag/AgCl在 +1100 mV下操作。在这些色谱条件下，药物在不到12分钟内洗脱。该方法在4.5 - 15μg/ml范围内呈线性，日内和日间重复性以相对标准偏差（R.S.D.）计低于15%，准确度大于98%，检测限从90 ng/ml（氨氯地平）到1.55μg/ml（尼群地平）不等。该方法成功应用于市售药品，相对误差低于5%。通过将所得结果与带光度检测的高效液相色谱法的结果进行比较，检验了该方法的有效性。
