摘要
目的 建立测定人体血浆苯磺酸左旋氨氯地平浓度的反相高效液相色谱测定法(RP-HPLC)。方法 采用C8色谱柱(4.6mm×150mm,5μm),以甲醇:20mmol·L^-1磷酸二氢钾(KH2P04)缓冲液(pH值3.5)=42:58为流动相.地尔硫[艹卓]为内标;流速:1.0mL·min^-1;血浆样品用甲醇沉淀蛋白,使用冷冻干燥的方法将样品浓缩,然后进样,进样量:50μL;紫外检测波长为238nm。结果 苯磺酸左旋氨氯地平浓度在0.2~20.0ng·ml^-1范围内线性关系良好(r=0.9987),平均绝对回收率为94.3%±4.6%(n=15),日内与日间精密度均≤9.6%。最低检测限为0.1ng·mL^-1;内源性物质不干扰测定。结论 该方法工作曲线稳定,灵敏度高,操作步骤简单。可以用于苯磺酸左旋氨氯地平的药动学研究及临床血药浓度监测。
Objective To set up an RP-HPLC method for the determination of the concentration of (S)-amlodipine benzenesulfonate in human blood plasma. Methods A reverse phase C8 column(4.6 mm×150 mm,5μm) served as the solid phase, the mobile phase was methanol -20 mmol·L^-1 potassium dihydrogen phosphate solution( pH = 3.5 ) ,42 : 58, V/V. with dihiazem as the internal standard ; the detection wavelength, 238 nm ; the flow rate, 1.0 mL· min^-1. The plasma samples were treated with methanol for the precipitation of protein and concentrated by freeze drying before addition to the system. The volume of samples added was 50μL. Results The calibration curve exhibited an excellent linear relationship with a correlation coefficient of 0. 998 7 when the concentration of (S)-amlodipine benzenesulfonate was within a range of 0.2~20.0 ng·mL^-1. The average absolute recovery rate was ( 94.3± 4.6 ) % ( n = 15 ). The within day and inter days preeisions (RSD) were both less than 9. 6%. The lower limit of detection was 0. 1 ng·mL^-1. The assay was not interfered with by endogenous substances. Conclusion The method was shown to be simple, sensitive and accurate and may be used in the pharmacokinetic and pharmacodynamic studies of (S)-amlodipine benzenesulfonate as well as in the monitoring of the blood concentration of the substance in the clinical practice.
出处
《医药导报》
CAS
2006年第12期1256-1259,共4页
Herald of Medicine