固相萃取RP-HPLC法测定西达本胺血药浓度  

Determination of Chidamide in Plasma by RP-HPLC with Solid-phase Extraction

作　　者：王欣[1] 孟湘明[1] 孟志云[1] 窦桂芳[1] 

机构地区：[1]中国人民解放军军事医学科学院野战输血研究所,北京100850

出　　处：《解放军药学学报》2006年第2期113-115,共3页Pharmaceutical Journal of Chinese People's Liberation Army

摘　　要：目的 建立测定西达本胺血药浓度的固相萃取RP-HPLC法。方法 采用Kromasil KR100-5C18（4．6mm×250mm，5μm）分析柱：柱温为室温；以0．6％醋酸水溶液．乙腈（0～6min，81：19和6—13min，76：24，v／v）为流动相，梯度洗脱；流速为1．0ml／min；紫外检测波长为260nm；以MS-275为内标，血浆样品用Waters OASIS固相萃取（SPE）小柱提取纯化，乙腈洗脱，吹干，用流动相复溶后进样分析，进样量20μl。结果 西达本胺血药浓度在0．04～10μg·ml^-1范围内线性关系良好（r=0．998 1），最低定量浓度为0．04μg·ml^-1。低、中、高3个浓度的日内RSD为5．79％～10．16％，日问RSD为2．01％～14．81％；RE为-0．85％～4．39％；平均回收率为74％。结论　此方法较简便、准确、精密度好，可以用做西达本胺的毒代动力学研究，并为临床前药代动力学研究打下了方法学基础。Aim To establish an RP-HPLC method for the determination of Chidamide in plasma. Method The Chi-damide with the internal standard MS-275 added was extracted from the plasma with a solid-phase extraction column. Theplasma sample was loaded onto a SPE column. The Chidamide was eluted with Acetonitrile, dried by air and determinedby reversed-phase high-performance liquid chromatography（RP-HPLC） at 260nm. The mobile phase consisted of 0.6%acetic acid solution and Acetonitrile（0 ～ 6min,81：19;6 ～ 13min,76：24） with the flow rate of 1.0ml/min. The columnwas KR100-5C18（4.6mm × 250mm,5μm）. The column temperature was room temperature, and the injected volume was20μl. Results The linear range was 0.04 ～ 10μg·ml^-1（ r = 0.998 1 ）, and the LLOQ was 0.04μg·ml^-1. The intra-dayand inter-day RSD were 2.01%（14.81% and 5.79% ～ 10.16% ,respectively. The RE was -0.85% ～ 4.39% .Theaverage extraction recovery was 74%. Conclusion The proposed method is simple, accurate and precise. It is suitable fortoxicokinetics study.

关 键 词：西达本胺 高效液相色谱法 固相萃取 血药浓度 

分 类 号：R927[医药卫生—药学]