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目的:建立同时测定患者血清中茶碱和多索茶碱浓度的HPLC法。方法:采用液-液萃取法对血样进行预处理,以咖啡因为内标。色谱条件Hypersil BDS C18柱(150mm×4.6mm,5μm,柱号:E1515982);流动相为甲醇-水(25∶75);流速为1.0mL.min-1;柱温为30℃,检测波长为紫外273nm。结果:在0.74~23.60mg.L-1范围内,茶碱血清浓度与茶碱和内标峰面积之比呈良好的线性关系,回归方程为Y=5.678 8X-0.025 8(r=0.999 7);在0.73~23.40mg.L-1范围内,多索茶碱血清浓度与多索茶碱和内标峰面积之比呈良好的线性关系,回归方程为Y=9.383 0X+0.085 5(r=0.999 9)。在本实验条件下,茶碱和多索茶碱的平均绝对回收率均达到80%左右,平均相对回收率分别为98.4%~100.8%,98.9%~101.5%,日内和日间RDS均小于10%。结论:该方法准确、经济、无杂质干扰,适用于茶碱和多索茶碱血药浓度监测及药动学研究。
Objective: To establish an HPLC method for the simultaneous determination of theophylline and doxofylline in serum of patients. Methods: Blood samples were pretreated by liquid - liquid extraction, with caffeine as internal standard. Chromatographic conditions Hypersil BDS C18 column (150mm × 4.6mm, 5μm, column number: E1515982); the mobile phase was methanol-water (25:75); the flow rate was 1.0mL.min-1; UV 273nm. Results: In the range of 0.74 ~ 23.60 mg.L-1, there was a good linear relationship between theophylline serum concentration and the peak area of theophylline and internal standard. The regression equation was Y = 5.678 8X-0.025 8 (r = 0.999 7) ; In the range of 0.73 ~ 23.40 mg.L-1, the relationship between doxofylline serum concentration and the peak area of doxofylline and internal standard showed a good linear relationship, the regression equation was Y = 9.383 0X + 0.085 5 (r = 0.999 9). Under the experimental conditions, the average absolute recovery of theophylline and doxofylline reached about 80%, the average relative recoveries were 98.4% ~ 100.8%, 98.9% ~ 101.5%, RDS were less than 10 day and day %. Conclusion: This method is accurate, economical and has no impurity interference. It is suitable for the monitoring of plasma concentration of theophylline and doxofylline and pharmacokinetics.