Development and validation of a liquid chromatographic method for the determination of amlodipine residues on manufacturing equipment surfaces.
Development and validation of a liquid chromatographic method for the determination of amlodipine residues on manufacturing equipment surfaces.
复制标题
开发和验证用于测定制造设备表面上氨氯地平残留的液相色谱方法。
DOI：
10.1016/s0731-7085(03)00109-2
复制
发表时间：
2003
影响因子：
3.4
通讯作者：
A. Ceccato
中科院分区：
文献类型：
--
作者：
R. Klinkenberg;B. Streel;A. Ceccato
在制药工业中，一个重要的步骤是从相关设备和区域中去除可能的药物残留物。清洁程序必须经过验证，因此必须特别注意确定痕量药物的方法。为了控制清洁程序，开发并验证了用于测定拭子样本中残留物的高效液相色谱法。为了从不锈钢中获得合适的回收率，对抽汲程序进行了优化。当使用两个用甲醇润湿的拭子时，平均回收率接近90%。在RP-18固定相上，使用由乙腈、甲醇和pH 3.0三乙胺溶液（15：35：50 v/v/v）组成的移动的相，在25 ℃下以等度模式对残留的乙腈进行色谱分析。在237 nm处进行UV检测。该方法在0.39 - 1.56 μg/ml浓度范围内具有选择性和线性。并对方法的准确度和精密度进行了研究。检测限和定量限分别为0.02和0.08 μg/ml。还研究了在取样程序的不同步骤中的稳定性和擦拭程序的精密度。
In the pharmaceutical industry, an important step consists in the removal of possible drug residues from the involved equipments and areas. The cleaning procedures must be validated and the methods to determine trace amounts of drugs have therefore to be considered with special attention. A high performance liquid chromatographic method for the determination of amlodipine residues in swab samples was developed and validated in order to control a cleaning procedure. The swabbing procedure was optimized in order to obtain a suitable recovery of amlodipine from stainless steel. A mean recovery close to 90% was obtained when two swabs moistened with methanol were used. The residual amlodipine was chromatographed at 25°C in the isocratic mode on a RP-18 stationary phase using a mobile phase consisting of acetonitrile, methanol and pH 3.0 triethylamine solution (15:35:50 v/v/v). UV detection was performed at 237 nm. The method was shown to be selective and linear into the concentration range varying from 0.39 to 1.56 μg/ml. Accuracy and precision of the method were also studied. The limits of detection and quantitation were evaluated to be 0.02 and 0.08 μg/ml, respectively. The stability of amlodipine at different steps of the sampling procedure and the precision of the swabbing procedure were also investigated.