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目的 :建立反相高效液相色谱法测定血浆中西沙必利浓度方法。方法 :采用LunaC18不锈钢分析柱 ,以 0 .0 2mol·L-1磷酸 乙腈 (6 2∶38,用浓氨水调pH至 6 .2 )为流动相 ,卡马西平作内标。样品在碱性条件下用含 5 %异戊醇的正庚烷旋涡混合萃取浓集后进样 ,在 2 73nm波长下检测 ,按内标法定量。结果 :标准曲线在 0 .5～ 12 8μg·L-1范围内有良好线性 ,最低检测浓度为 0 .3μg·L-1,方法回收率为 92 %～ 10 3 % ,日内RSD小于 2 .5 % ,日间RSD小于 5 .5 %。结论 :本法具有快速简便 ,灵敏准确等特点 ,已用于西沙必利片剂及胶囊剂的生物利用度测定 ,结果良好。
Objective: To establish a method for the determination of cisapride in plasma by reversed-phase high performance liquid chromatography. Methods: Luna C18 stainless steel was used as the mobile phase. The mobile phase consisted of 0. 02 mol·L-1 phosphoric acid and acetonitrile (6:38, adjusted to pH6.2 with concentrated aqueous ammonia). Carbamazepine was used as internal standard. The sample was concentrated with n-heptane vortex containing 5% isoamyl alcohol under alkaline conditions and injected into the sample. The sample was detected at a wavelength of 273 nm and was quantified by internal standard method. Results: The calibration curve showed a good linearity in the range of 0.5 ~ 12.8μg · L-1 with the lowest detection concentration of 0.3μg · L-1, the recovery rate was 92% -103% and the intra-day RSD was less than 2.5 %, Daytime RSD less than 5.5%. Conclusion: This method has the characteristics of quick and easy, sensitive and accurate, has been used in the determination of bioavailability of cisapride tablets and capsules with good results.