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目的 :建立人血浆中西沙必利的高效液相色谱测定法。方法 :取血浆 2 0 0 μL ,碱化后用正庚烷 -异戊醇 (95∶5 )一步提取 ,常温下氮气吹干。采用Shim -packCLC -ODS色谱柱 ;流动相为磷酸二氢钾溶液 (pH =4 5 ,0 0 2mol·L- 1 ) -乙腈=5 7∶43,流速 1 3mL·min- 1 ;检测波长 315nm ;柱温 35℃。结果 :西沙必利与内标物的保留时间分别为 4 0min和 5 4min ;西沙必利浓度C在 4～ 2 0 0 μg·L- 1 范围内与西沙必利 内标物的峰高比PHR呈良好线性关系 ,回归方程为 :PHR =0 0 0 8193C +0 0 0 2 75 4,r=0 9997,n =9,,斜率RSD =4 82 %。高中低 3个质控样本的批内 (n =10 )及批间 (n =9)RSD分别为 2 91%～ 3 5 7%和 3 30 %～ 3 99% ,方法学回收率为 96 %～ 10 0 % ,最低可检出浓度为 2 μg·L- 1 。除妥拉苏林外 ,西沙必利代谢物Norcisapride及其它被测药物对西沙必利和内标物均无干扰。结论 :本方法取样量小、灵敏度高、操作便捷 ,为血药浓度监测及临床药代动力学研究提供了方法学基础。
Objective: To establish a HPLC method for the determination of cisapride in human plasma. Methods: Take 200 μL of plasma and alkalize it, then extract it with n-heptane-isopentyl alcohol (95: 5) in one step and dry it by nitrogen at room temperature. The mobile phase was potassium dihydrogen phosphate (pH = 4.5, 0.02 mol·L-1) -acetonitrile = 5 7:43, the flow rate was 13 mL · min-1 and the detection wavelength was set at 315 nm ; Column temperature 35 ℃. Results: The retention times of cisapride and internal standard were 40 min and 54 min, respectively. The peak height-height ratio of cisapride concentration C to cisapride internal standard in the range of 4 ~ 200 μg · L-1 PHR The regression equation was: PHR = 0 0 0 8193C + 0 0 0 2 75 4, r = 0 9997, n = 9, slope RSD = 4 82%. The intra-assay (n = 10) and inter-batch (n = 9) RSDs for high, middle and low quality control samples ranged from 2191% to 375% and from 30% to 39%, respectively. The methodological recovery was 96% ~ 10 0%, the lowest detectable concentration of 2 μg · L- 1. In addition to tora Suurin, norcisapride, a metabolite of cisapride, and other drugs tested showed no interference with cisapride and internal standard. Conclusion: The method of small sample volume, high sensitivity, easy to operate, for the blood concentration monitoring and clinical pharmacokinetic studies provide a methodological basis.