Zaater M, Hasan E, Najib N
Department of Applied Chemistry, Jordan University of Science and Technology Irbid.
Pol J Pharmacol. 2000 Jul-Aug;52(4):307-12.
A rapid, simple, specific and sensitive high performance liquid chromatographic method has been developed for the determination of nifedipine (adalate) in human serum using diazepam (valium) as an internal standard (I.S.). The method utilized a 5 microm nonpolar C18 reversed phase Hypersil (ODS) column (250 x 3 mm i.d.). The mobile phase consisted of 60% v/v, acetonitrile in water, adjusted to pH 3.7 with glacial acetic acid and ammonium acetate, and pumped at a flow rate of 2 ml/min. The effluent was monitored by UV detection at 340 nm and a sensitivity fixed at 0.02 aufs. Each analysis required no longer than 4 min. The minimum detectable amount of nifedipine in serum was 3 ng/ml, and the mean absolute recovery was 93.5%. The within and between-day coefficients of variation at three different concentrations from 15-160 ng/ml ranged from 2.07 to 7.76%, and from 3.15 to 7.98% respectively. Calibration graphs for 10 to 200 ng/ml were linear with a mean correlation coefficient, r (n = 36) of 0.9991. The method was validated for accuracy, sensitivity, selectivity and reproducibility and finally was utilized and proved to be suitable in a bioavailability study of two products of nifedipine following oral administration to healthy male subjects.
已开发出一种快速、简便、特异且灵敏的高效液相色谱法，以地西泮（安定）作为内标物，用于测定人血清中的硝苯地平（心痛定）。该方法采用一根5微米非极性C18反相Hypersil（ODS）柱（250×3毫米内径）。流动相由60%（v/v）乙腈与水组成，用冰醋酸和醋酸铵调至pH 3.7，以2毫升/分钟的流速泵送。流出物通过在340纳米处的紫外检测进行监测，灵敏度设定为0.02aufs。每次分析所需时间不超过4分钟。血清中硝苯地平的最低检测量为3纳克/毫升，平均绝对回收率为93.5%。在15 - 160纳克/毫升的三个不同浓度下，日内和日间变异系数分别在2.07%至7.76%以及3.15%至7.98%之间。10至200纳克/毫升的校准曲线呈线性，平均相关系数r（n = 36）为0.9991。该方法在准确性、灵敏度、选择性和重现性方面得到验证，最终用于健康男性受试者口服两种硝苯地平制剂的生物利用度研究，并证明是适用的。
