超高效液相色谱法测定人血浆中全反式维甲酸的浓度  

Determination of the concentration of all-trans retinoic acid in human plasma by ultra performance liquid chromatography

作　　者：程昱[1] 刘茂柏[1] 阙万才[1] 丘宏强[1] CHENG Yu;LIU Mao-bo;QUE Wan-cai;QIU Hong-qiang(Department of Pharmacy, Fujian Medical University Union Hospital, Fuzhou 350001,Fujian Province,China)

机构地区：[1]福建医科大学附属协和医院药学部

出　　处：《中国临床药理学杂志》2019年第13期1381-1383,1387,共4页The Chinese Journal of Clinical Pharmacology

基　　金：福建省科技创新联合基金资助项目(2017Y9036)

摘　　要：目的建立超高效液相色谱法测定人血浆中全反式维甲酸的浓度。方法用沉淀蛋白后固相萃取对血浆样本进行前处理后进样,色谱柱:Shim-pack GIST-HP C18柱(3μm,2. 1 mm×100 mm),流动相:甲醇-1%冰醋酸(80∶20),流速:0. 35 mL·min^-1,紫外检测波长:350 nm,柱温:25℃,进样量:50μL。结果全反式维甲酸血浆浓度在10~1000 ng·mL^-1具有良好的线性关系,回归方程为y=0. 73×10^-2x+0. 72×10^-2(r=0. 999 8),最低检测限为1. 5ng·mL^-1;平均提取回收率为(83. 88±2. 07)%,平均方法回收率为(94. 95±3. 13)%,日内精密度RSD≤3. 46%,日间精密度RSD≤6. 20%。稳定性结果显示灯光下放置8 h全反式维甲酸浓度降低(22. 93±8. 54)%,室温放置24 h、4℃放置24 h、-20℃冻存2周、-20℃反复冻融全反式维甲酸浓度基本保持稳定。结论本方法准确、快速、灵敏、重现性好,适用于全反式维甲酸临床血药浓度的监测。Objective To establish the methods for determination of all - trans retinoic acid in human plasma by ultra performance liquid chromatography. Methods After precipitated protein,the sample was exacted by Solid phase extraction cartridge. A Shim - pack GIST - HP C18 column ( 3 μm,2. 1 mm × 100 mm) was adopted. The mobile phase was methanol and 1% glacial acetic acid ( 80 ∶ 20). The flow rate was 0. 35 mL·min^-1,the injection volumn was 50 μL,the detection wavelength was set 350 nm,and the temeparature was 25 ℃. Results The method was linear in the range of 10 - 1000 ng·mL^-1,y = 0. 73 × 10^-2 x + 0. 72 × 10^-2 ( r = 0. 999 8). The detection limit was 1. 5 ng·mL^-1. The average recovery was ( 83. 88 ± 2. 07)%,and the recovery rate of the method was ( 94. 95 ± 3. 13)%. The intra - day RSD was ≤ 3. 46% and the intra - day RSD was ≤ 6. 20%. The stability test results showed that the concentrations of all - trans retinoic acid were reduced by ( 22. 93 ± 8. 54)% under the light condition,while the concentrations of all - trans retinoic acid remained stable at room temperature,refrigeration,freezing and freeze - thaw conditions. Conclusion The established method for the determination of all - trans retinoic acid in human plasma by ultra performance liquid chromatography is suitable for clinical therapeutic drug monitoring and pharmacokinetic study with its accurate,rapid and simple.

关 键 词：超高效液相色谱法 全反式维甲酸 血浆浓度 固相萃取 

分 类 号：R97[医药卫生—药品]