Klinkenberg R, Streel B, Ceccato A
Galephar M/F, 39, rue du Parc Industriel, B-6900 Marche-en-Famenne, Belgium.
J Pharm Biomed Anal. 2003 Jun 1;32(2):345-52. doi: 10.1016/s0731-7085(03)00109-2.
In the pharmaceutical industry, an important step consists in the removal of possible drug residues from the involved equipment 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 degrees 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 microg/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 microg/ml, respectively. The stability of amlodipine at different steps of the sampling procedure and the precision of the swabbing procedure were also investigated.
在制药行业，一个重要步骤是清除相关设备和区域中可能存在的药物残留。清洗程序必须经过验证，因此对于测定痕量药物的方法必须给予特别关注。为了监控一个清洗程序，开发并验证了一种用于测定拭子样品中氨氯地平残留量的高效液相色谱法。对拭子取样程序进行了优化，以便从不锈钢表面获得合适的氨氯地平回收率。当使用两根用甲醇浸湿的拭子时，平均回收率接近90%。残留的氨氯地平在25℃下，以等度洗脱模式在RP - 18固定相上进行色谱分析，流动相由乙腈、甲醇和pH 3.0的三乙胺溶液（15:35:50 v/v/v）组成。在237 nm波长处进行紫外检测。该方法在0.39至1.56微克/毫升的浓度范围内具有选择性和线性。还研究了该方法的准确度和精密度。检测限和定量限分别评估为0.02和0.08微克/毫升。还研究了氨氯地平在取样程序不同步骤的稳定性以及拭子取样程序的精密度。
