摘要
目的:建立反相高效液相色谱内标法测定人血浆中枸橼酸坦度螺酮的浓度。方法:枸橼酸坦度螺酮血浆样品加入奥卡西平内标液,经2 mol·L^(-1)碳酸钠碱化后用乙酸乙酯-正己烷(4:1)一步提取,上清液于50℃水浴氮气吹干。色谱柱:Hyper-sil C_(18)(4.6 mm×250 mm,5μm,Agilent);流动相:乙腈-水-0.15 mol·L^(-1)磷酸二氢钠缓冲液(pH=3.0)(33:62:5);流速:0.8 mL·min^(-1);检测波长:239 nm;柱温:35℃。结果:枸橼酸坦度螺酮在0.02~5.0μg·mL^(-1)范围内线性关系良好(r=0.9994),定量下限为0.02μg·mL^(-1)。相对回收率98.6%~99.8%,提取回收率83.2%~92.3%,日内和日间 RSD 分别为2.9%~4.9%和3.8%~5.1%。结论:本法简便、准确、灵敏度高,适用于枸橼酸坦度螺酮的临床血药浓度检测及药代动力学研究。
Objective:To establish an RP - HPLC method for the determination of tandospirone citrate in human plasma. Methods: After addition of oxcarbazepine ( internal standard ) , tandospirone citrate was extracted from human plasma with ethyl acetate - n-hexane (4:1 )after alkalified by 2 mol·L^-1 Na2 CO3, the supernatant was evaporated at 50℃. The analytical column was packed with Hypersil C18 (4.6 mm ×250mm,5μm,Agilent). The mobile phase was acetonitrile - water - 0. 15 mol·L^- 1 NaH2PO4 solution ( pH = 3.0 ) ( 33 : 62 : 5 ), the flow rate was 0.8 mL· min^-1 ,the UV absorbanee wavelength was 239 nm ,and the column temperature was 35 ℃. Results :The calibration curve was in good linearity in the range of 0.02 - 5.0μg·mL^-1 ( r = 0. 9994 ). The quantitation limit was 0.02 μg·mL^-1. The relative recovery of method was 98.6% -99. 8%. The extraction recovery was 83.2% - 92.3%. Within - day precision (RSD) was 2.9% -4.9%, between - day precision (RSD) was 3.8% - 5. 1%. Conclusion: The method is convenient, accurate, sensitive, and is suitable for the determination of tandospirone citrate in human plasma and pharmacokinetic studies.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2006年第12期1751-1753,共3页
Chinese Journal of Pharmaceutical Analysis