Alsarra Ibrahim A
Department of Pharmaceutics, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh 11451, Saudi Arabia.
J Chromatogr Sci. 2009 Nov-Dec;47(10):863-7. doi: 10.1093/chromsci/47.10.863.
An accurate, sensitive, and reproducible high-performance liquid chromatographic method for the quantitation of amlodipine besylate in human plasma has been developed and validated. The drug, internal standard, and major metabolite were eluted from a C(18) hypersil HyPurity column (3 microm, 3.9 mm i.d. x 150 mm) at room temperature with a mobile phase consisting of acetonitrile-potassium dihydrogen phosphate buffer (0.05 M) and acetic acid (62:38:0.1) with the pH adjusted to 3.5 using phosphoric acid. The flow-rate was 1.8 mL/min. The limit of detection was 1.0 ng/mL, and the limit of quantification of amlodipine besylate in plasma was 10 ng/mL. The intra- and inter-day precisions showed coefficients of variation ranging from 5.98-11.4% and from 5.60-11.74%, respectively at three different levels of concentration. The averages of the absolute and relative recoveries were found to be 96.74-98.51% and 95.96-100.71%, respectively. Stability studies showed that amlodipine besylate is stable for at least 2 months in plasma after freezing at -20 degrees C. The method was successfully applied for a pharmacokinetic study and for the determination of commercial amlodipine tablet content.
已开发并验证了一种准确、灵敏且可重现的高效液相色谱法，用于定量测定人血浆中的苯磺酸氨氯地平。该药物、内标物和主要代谢物在室温下从C(18) 超纯HyPurity柱（3微米，内径3.9毫米×150毫米）上洗脱，流动相由乙腈-磷酸二氢钾缓冲液（0.05 M）和乙酸（62:38:0.1）组成，用磷酸将pH调至3.5。流速为1.8毫升/分钟。检测限为1.0纳克/毫升，血浆中苯磺酸氨氯地平的定量限为10纳克/毫升。日内和日间精密度在三个不同浓度水平下的变异系数分别为5.98 - 11.4%和5.60 - 11.74%。绝对回收率和相对回收率的平均值分别为96.74 - 98.51%和95.96 - 100.71%。稳定性研究表明，苯磺酸氨氯地平在-20℃冷冻后在血浆中至少稳定2个月。该方法已成功应用于药代动力学研究和市售氨氯地平片剂含量的测定。
