论文部分内容阅读
目的 :建立水溶性药物呱仑酸钠血药浓度的高效液相色谱分析方法。方法 :以对二甲氨基苯甲醛为内标 ,在比较了固相萃取、离子对萃取及沉淀蛋白 -脱水法等 3种预处理方法的基础上 ,采用沉淀蛋白 -脱水法预处理兔血浆样品 ,分析柱为 μBondapakC18柱 (2 5 0mm× 4 6mm ,10 μm) ,流动相为 pH 7 0的 0 0 1mol·L-1磷酸盐缓冲液 -甲醇 (5 0∶5 0 ) ,流速1mL·min-1,在 2 93nm波长处检测 ,按内标法定量。结果 :血药浓度线性范围为 0 1~ 10 0mg·L-1(r=0 9997) ,最低检测浓度为 0 0 2mg·L-1(S/N >3) ,萃取回收率在 79 5 %~ 86 4% (n =5 ) ,分析方法回收率在 93 1%~ 95 5 % (n =5 ) ,日内和日间RSD分别为 1 2 %~ 1 8%和 1 9%~ 3 1% (n =5 )。结论 :本法简便、准确、精密度高、重现性好 ,适用于呱仑酸钠的体内研究
Objective: To establish a high performance liquid chromatographic method for the determination of the drug concentration of sodium valproate in water. Methods: The p-dimethylaminobenzaldehyde was used as an internal standard. Based on three pretreatment methods, solid phase extraction, ion-pair extraction and precipitated protein-dehydration, pretreatment of rabbit plasma samples . The analytical column was μ Bondapak C18 column (250 mm × 4 6 mm, 10 μm) with a mobile phase of 0 0 1 mol·L-1 phosphate buffer-methanol (50:50) at a pH of 70 and a flow rate of 1 mL · min -1, detected at 2 93nm wavelength, quantified by internal standard method. Results: The linear range of plasma concentration was 0 1 ~ 100 mg · L-1 (r = 0 9997), the lowest detection concentration was 0 0 2 mg · L-1 (S / N> 3) (N = 5). The recovery rates of the analytical methods ranged from 93 1% to 95 5% (n = 5) with daily and daily RSDs of 12% ~ 18% and 19% ~ 31% (n = 5). Conclusion: This method is simple, accurate, high precision, reproducible, suitable for in vivo study of sodium gound