反相高效液相色谱法测定人血清中比卡鲁胺浓度

RP-HPLC determination of bicalutamide in human serum

目的:建立测定比卡鲁胺血药浓度的高效液相色谱法。方法:以固相萃取法对血样进行预处理。用反相高效液相色谱-紫外检测法测定人血中比卡鲁胺,采用 Waters Symmetry C_(18)色谱柱(150 mm×4.6 mm,3.5 μm),流动相为0.1%磷酸二氢钾-乙腈(50:50),流速1 mL·min^(-1),检测波长272 nm,柱温25℃。结果:比卡鲁胺浓度在0.013～1.300μg·mL^(-1)范围内线性良好(r=0.9993);方法的最低检测限为0.0013μg·mL^(-1)(S/N=3);低、中、高3种浓度的绝对平均回收率分别为95.0%±3.2%,97.8%±1.8%,97.5%±0.5%;相对平均回收率分别为99.1%±4.0%,107.0%±2.0%,99.3%±0.2%;低、中、高3种浓度的日内、日间 RSD(n=5)分别为4.77%,1.03%,0.38%和5.46%,1.77%,0.47%。结论:此方法操作简便,灵敏,准确,适用于比卡鲁胺的临床药代动力学研究。

Objective ：To establish an HPLC method for the determination of bicalutamide in human serum. Methods ：The serum samples were pretreated by solid -phase extraction method and bicalutamide was determined by HPLC -UV. Waters Symmetry Cls chromatographic column （150 mm ×4.6 mm,3.5 μm） was used and the mobile phase consisted of 0. 1% potassium dihydrogen phosphate - acetonitrile （50： 50） with a flow rate of 1 mL· min ^- 1, the detection wavelength was set at 272 nm and the temperature of the column was controlled at 25 ℃. Results： The calibration curve was linear within the range of 0. 013 to 1. 300 μg · mL^-1 （r =0. 9993）. The lowest limit of detection was 0. 0013 μg · mL^-1（ S/N = 3 ）. The mean absolute and relative recovery for three concentration of bicalutamide were 95.0% ±3.2% ,97.8% ± 1.8% ,97.5% ±0. 5% and 99. 1% ±4.0% ,107.0% ±2. 0% ,99.3% ± 0. 2% ,respectively. Intra -day and inter -day RSD （n =5） were 4.77% ,1.03% ,0. 38% and 5.46% ,1.77%, 0. 47% ,respectively. Conclusion：The method is simple, sensitive, accurate, reproducible and suitable for the clinical pharmacokinetic study of bicalutamide.