中空纤维超滤-高效液相色谱法测定人血浆中的阿昔莫司

Determination of acipimox in human plasma by ultrafiltration-high performance liquid chromatography with hollow fiber

目的建立中空纤维超滤-高效液相色谱测定人血浆中阿昔莫司浓度的方法。方法用中空纤维离心超滤除去样品溶液中的大分子;色谱柱为InertsilODS-3;流动相为A:水-冰醋酸(28∶1),B:甲醇,A∶B(99∶1);流速为1.0 mL.min-1;柱温为30℃;检测波长275 nm。结果当阿昔莫司血药浓度在0.25～16.00μg.mL-1内线性关系良好(r=0.999);高、中、低3个浓度的回收率分别为107.5%,105.6%,104.5%;日内、日间精密度的RSD均小于8%;稳定性均良好。结论本法简便、灵敏、回收率高,重现性好,可用于患者的血药浓度监测和药代动力学研究。

Objective To establish a hollow fiber ultrafihration - HPLC method for the determination of acipimox in human plasma. Methods Hollow fiber was used to remove the maeromolecule in sample solution. The content of acipimox was detected by ultraviolet detector at 275 nm with Inertsil ODS - 3 column at a flow rate of 1.0 mL · min - 1. A phase was water - glacial acetic acid （ 28 ： 1 ） , B phase was methanol. The mobile phase was A phase - B phase（99：1 ）. The column temperature was 30 ℃. Results The linear range was 0.25 - 16.00 μg · mL- 1 （ r = 0. 999 ）. The average absolute recovery was 107.5 % , 105.6 % , 104.5 % for the high, middle, low control sam- ples. The relative standard deviation obtained for inter- and intra - assay precisions were both less than 8%. Conclusion This method is convenient, sensitive and reproducible, suitable for the determination of acipimox in human plasma for pharmacokinetics and monitoring acipimox concentration in patient.