摘要
目的:建立固相萃取反相高效液相色谱法测定人血清中托烷司琼的浓度。方法:采用 Waters Oasis HLB 萃取小柱对血清样品进行固相萃取,以昂丹司琼为内标,在 Waters 高效液相色谱系统上,C_(18)为固定相,乙腈-50mmol·L^(-1)磷酸盐缓冲液(20:80,pH5.0,含0.3%三乙胺)为流动相,流速:1mL·min^(-1),检测波长:285nm。结果:托烷司琼和内标物洗脱时间分别为5.3min 和6.9min,与血中内源性杂质得到良好分离。方法的相对回收率为98.9%±1.0%,日内日间变异 RSD 范围分别为0.9%～5.3%和2.99%～4.2%,线性范围为0.5～64.0ng·mL^(-1),当 S/N≥3时,托烷司琼最低检出浓度可达0.5ng·mL^(-1)。结论:所建方法准确、灵敏,可满足血药浓度监测和药代动力学参数测试的需求。
Objective： To establish an RP - HPLC with solid - phase extraction method for determination of tropisetron（Trop） concentration in human serum. Methods： Using ondansetron as an internal standard（IS）, solid- phase extraction of human serum with Waters Oasis HLB column. The Trop and IS were separated on the Waters Symmetry C 18 column with acetonitrile- 50 mmol · L^-1 phosphate buffer of pH 5.0 （20： 80,0. 3% triethylamine） as the mobile phase, a flow rate of 1 mL · min^-1 and detected at 285 nm, column temperature at 30 ℃. Results： The linear rang of calibration curve was within drug serum concentrations of 0. 5 - 64 ng · mL^-1 （ n = 8, r = 0. 9999）. The lower limit of quantification（S/N≥3） was 0. 5 ng· mL^-1. Intra- and inter- assay RSD ranged from 0. 9% to 5.3% and 2. 9% to 4. 2%. Mean recovery was 98.9% ± 1.0%. Conclusion： ：The method can be used for detection of tropisetron concentration in human serum and the estimation of pharmacokinetic parameters.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2006年第2期184-187,共4页
Chinese Journal of Pharmaceutical Analysis
