摘要
目的:建立反相高效液相色谱法测定大鼠血清中蟾蜍灵浓度。方法:血清样品用乙醚-乙酸乙酯(5:1)提取两次,40℃水浴氮气吹干,残留物用甲醇溶解后进样。色谱柱为Shim-pack VP-ODS柱(4.6 mm×150mm,5 μm),流动相为甲醇-水(70:30),流速1.0 mL·min～1,紫外检测波长298 nm,柱箱温度30℃。内标物为华蟾酥毒基。结果:本法最低检测浓度为0.05μg·mL～1,线性范围为0.1-1.6μg·mL-1,r=0.9977。日内精密度RSD小于4%,日间RSD小于10%,蟾蜍灵的萃取回收率为84.0%。结论:本法快速、准确、灵敏,可用于蟾蜍灵的体内药物动力学研究。
Objective:To establish a method for the determination of bufalin in rat serum using RP - HPLC. Methods; The serum samples were extracted twice with ether - ethyl acetate(5: 1). The solvent was evaporated to dryness under a gentle stream of N2 at 40 ℃ in a water bath. The analysis involved a shim - pack VP - ODS column(150 mm ×4. 6 mm, 5 μm)as stationary phase and methanol -water (70= 30) as mobile phase. The flow rate was 1. 0 mL · min -1, UV detection wavelength was at 298nm and the column temperature at 30 ℃. Cinobufagin was used as the internal standard. Results:The minimal detectable drug serum concentration was 0. 05 μg · mL-1 . The calibration curve was linear in range of 0. 1 μg · mL-1 to 1. 6 μg · mL-1. Inter - day precision RSD was less than 4% and in-tra - day less than 10% , respectively. The absolute recovery of bufalin was 84. 0%. Conclusion; This method is economic, simple, rapid, sensitive and accurate. It can be used for the study on the pharmacokinetics of bufalin.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2004年第5期523-525,共3页
Chinese Journal of Pharmaceutical Analysis
基金
天津市自然科学基金资助课题(批准号013804311)
