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目的建立高效液相色谱-荧光检测法测定小鼠全血中格拉司琼浓度的方法,考察方法的专属性、线性关系、准确度、精密度、稳定性、提取回收率等效能指标。方法采用腈基柱;流动相:磷酸三乙胺缓冲盐溶液-乙腈(85∶15 v/v);检测波长:λex=302 nm,λem=360 nm;柱温26℃;流速1.0 ml/min;进样量20μl。生物样品预处理采用氢氧化钠碱化,二氯甲烷:乙醚(2∶3)萃取。结果小鼠全血中格拉司琼在0.5~50.0 ng/ml浓度范围内线性关系良好,回归方程为Y=5.35×102X+6.40×102,r=0.9968。本方法在低、中、高3个浓度质控样品的日内精密度分别为7.32%,4.74%,6.86%,日间精密度分别为11.2%,13.03%,7.68%;提取回收率均在76%以上。结论高效液相色谱-荧光检测法测定血中格拉司琼浓度简便、快速、准确、专属性强。
OBJECTIVE To establish a method for the determination of granisetron in mouse whole blood by high performance liquid chromatography-fluorescence detection and investigate the specificity, linearity, accuracy, precision, stability and extraction recovery of the method. The mobile phase was triethylamine phosphate buffered saline-acetonitrile (85:15 v / v). The detection wavelength was λex = 302 nm, λem = 360 nm. The column temperature was 26 ℃. The flow rate was 1.0 ml / min ; Injection volume 20μl. Biological samples were pretreated with sodium alkalisation and extracted with dichloromethane: ether (2: 3). Results Granisetron in whole blood of mice showed a good linearity in the concentration range of 0.5-50.0 ng / ml. The regression equation was Y = 5.35 × 102X + 6.40 × 102, r = 0.9968. The intra-day precision of this method was 7.32%, 4.74%, 6.86% in the low, middle and high quality control samples respectively, and the intra-day precision was 11.2%, 13.03% and 7.68% %the above. Conclusion The determination of granisetron in blood by high performance liquid chromatography with fluorescence detection is simple, rapid, accurate and specific.