摘要
建立了一种简便、灵敏、可重复的高效液相色谱法检测水牛血浆中吡喹酮(Praziquantel,PZQ)的含量。吡喹酮在C18(250mm×4.0mm,5μm)柱中可以很好地与杂质峰分离开。其保留时间、紫外检测波长、流动相、流速、色谱柱温度分别为10.6min、220nm、甲醇:水(70:30,V/V)、0.8mL/min和40℃。水牛血浆样品(0.5mL)经乙酸乙酯(6mL)两步提取后,采用旋转蒸发仪蒸干,1mL流动相溶解定容,取上清滤液20汕L进样做HPLC分析。吡喹酮的血浆药物浓度在0.0625~8mg/L范围内,呈现良好的线性关系,相关系数r〉0.999。在0.0625、1、16mg/L的3个药物浓度水平下,吡喹酮的平均回收率均在90%以上。日内和日间变异系数小于5%。PZQ的LOD可达0.01mg/L,LOQ为0.03mg/L。该方法的专属性强、灵敏度高,适用于水牛血浆中PZQ的药动学检测。
A simple, sensitive and reproducible method based on a reversed -phase chromatography was developed for the determination of praziquantel in water buffalo plasma. Praziquantel was separated from the impurities on a C18 column (250 mm × 4.0 mm, 5 μm) ,with retention times of 10.6 rain. Ultraviolet detection was set at 220 nm. The mobile phase consisted of methanol and distilled water (70 : 30, V/V) , running through the column at a flow rate of 0.8 mL/min. The chromatographic analysis was operated at 40℃. Sample preparation (0.5 mL plasma) was done by a single step liquid- liquid extraction with ethyl acetate. Calibration curves in plasma at the concentrations ( 0. 062 5 - 8 mg/L) were all linear with correlation coefficients higher than 0. 999. At the fortified levels of 0. 062 5,1,16 mg/L, the mean recoveries of PZQ ranged from 90% to 120%. The precision of the method based on within - day repeatability and reproducibility ( day - to - day variation ) was below 5%. Limit of detection (LOD) was 0.01 mg/L. LOQ was 0. 03 mg/L. The method was applicable to pharmaeokinetics detection of PZQ in water buffalo plasma.
出处
《中国兽药杂志》
2010年第3期9-12,共4页
Chinese Journal of Veterinary Drug
基金
中国农业科学院上海兽医研究所资助项目