RP-HPLC柱前衍生化法测定白舒非血药浓度  

Determination of Human Plasma Concentration of Busulfan by Pre-column Derivatization RP-HPLC

作　　者：王来成[1] 云筠筠[1] 胡丽丽[1] 李振宇[2] 董超[1] 韩强[1] 吕冬梅[1] 邵珠民[1] 

机构地区：[1]徐州医学院附属医院药剂科,江苏徐州221006 [2]徐州医学院附属医院血液科,江苏徐州221006

出　　处：《肿瘤药学》2012年第4期312-316,共5页Anti-Tumor Pharmacy

基　　金：江苏省卫生厅奥赛康临床药学研究基金项目资助(P200963)

摘　　要：目的建立测定人血浆中白舒非浓度的柱前衍生高效液相色谱法。方法以1,5-戊二醇二甲磺酸酯为内标,血浆样品经二乙基二硫代氨基甲酸钠衍生化处理后,以乙腈-0.7%冰醋酸水溶液(69∶31)为流动相,流速1.0mL·min-1,采用XterraP18色谱柱分离,在280nm波长下进行检测。结果白舒非线性范围为0.20～4.00mg·L-1,以加权最小二乘法计算得到回归方程为Y=2.56X+16.7(r=0.9993,n=7),提取回收率81.01%～82.72%,方法回收率96.50%～97.90%,日内、日间精密度(RSD)均小于10%。最低血浆检测质量浓度为0.080mg·L-1。结论柱前衍生高效液相色谱法准确、灵敏,适用于白舒非血浆浓度的测定及其药代动力学研究。Objective To develop a pre-column derivatization high performance liquid chromatography for detemfination of the plasma busulfan concentration. Methods 1,5-diol dimethyl sulfonate was used as internal standard, and plasma samples were processed by derivatization with sodium diethyldithiocarbamate, with acetonitrile -0.7 % acetic acid （69：31） as mobile phase, flow rate of 1.0 mL.min^-1, and separated by Xterra RP18 column （5 μm, 4.6 mm×250 mm）, then detected at 280 nm wavelength. Results The linear range of Bustfifan plasma concentration was 0.20-4.00 mg·L^- 1. Computing with the weighted least squares, the regression equation was Y=2.56X＋16.7 （r=0.9993, n=7）. The extraction recovery was 81.01% - 82.72% and the method recovery was 96.50% -97.90%. The intra-and inter-day RSD were less than 10%. The detected mininmm plasma concentration was 0.080 mg.L^-1. Conclusion This pre-colunm derivatization high perfomlance liquid chromatography is accurate, sensitive and suitable for deternfination of Busulfan plasma concentration and pharmacokinetic studies.

关 键 词：高效液相色谱法 白舒非 柱前衍生法 血药浓度 

分 类 号：R733.7[医药卫生—肿瘤] R917[医药卫生—临床医学]