摘要
目的 建立检测亚硫酸氢钠穿心莲内酯血浆浓度的反相离子对高效液相色谱 (Ion pairRP HPLC)法 ,研究亚硫酸氢钠穿心莲内酯在Beagle犬体内的药动学。 方法 血浆样品经含离子对试剂四丁基溴化铵的二氯甲烷萃取后 ,用 40℃氮气流吹干 ,残渣用流动相溶解后进行分析。流动相为甲醇∶0 0 9mol·L 1 磷酸二氢钾水溶液 (含四丁基溴化铵 6mmol·L 1 ) (4 5∶5 5 ) ,pH值 =7 2 5 ;固定相为Shim packVP ODS色谱柱 ;流速为 1.0mL·min 1 ;紫外检测波长 2 15nm ,室温 ,内标法定量。结果 线性范围为 1～ 3 0 0mg·L 1 ,最低检测浓度 0 0 5mg·L 1 ,平均回收率 96 44 % ,日内、日间精密度均 <5 0 % ,血浆在 -2 0℃下保存稳定。Beagle犬静脉注射亚硫酸氢钠穿心莲内酯后的药动学行为符合二室模型。结论 该检测方法准确、灵敏、简便 ,适用于亚硫酸氢钠穿心莲内酯血浆浓度的测定和药动学研究。亚硫酸氢钠穿心莲内酯在Beagle犬体内分布及消除较快。
Objective To set up an ion-pair reverse-phase high performance liquid chromatographic(Ion-pair RP-HPLC) method for the determination of plasma andrograpolide sodium bisulphite concentration and to study the pharmacokinetics of the drug after intravenous injection in beagle dogs. Methods Plasma samples were extracted with dichloromethane containing 3 mmol·L -1 of ion-pair reagent tetrabutyl ammonium bromide and dried with nitrogen gas flow at 40℃. The residue was then dissolved in the mobile phase and separated on a Shim-pack VP-ODS column(5μm, 150 mm×4.6 mm). The mobile phase was a mixture of methanol and 0.09 mol·L -1 monopotassium phosphate solution (45∶55) containing 6 mmol·L -1 of tetrabutyl ammonium bromide with the pH value adjusted to 7.25 with 1.0 mol·L -1 sodium hydroxide solution. The flow-rate was 1.0 mL·min -1 and the UV detection wavelength set at 215 nm. Quantitation was carried out with the internal standard method at room temperature . Results The calibration curve was shown to be linear within the range from 1 to 300 mg·L -1 and the within-day and between-day RSDs were all below 5%. The minimum detection concentration was 0.05 mg·L -1. The average recovery rate was 96.44%.The plasma andrographolide sodium bisulphite was stable at -20℃. After intravenous injections of 50, 40, 20 mg·kg -1 of andrographolide sodium bisulphite in beagle dogs, the concentration-time curve was fitted to a two compartment model. Conclusion The pharmacokinetics of andrographolide sodium bisulphite after IV administration showed a rapid distribution and elimination process in beagle dogs. The method was accurate, sensitive, simple and convenient for the measurement of plasma concentration and pharmacokinetic studies of andrographolide sodium bisulphite.
出处
《医药导报》
CAS
2005年第2期109-111,共3页
Herald of Medicine
关键词
亚硫酸氢钠穿心莲内酯
四丁基溴化铵
离子对萃取
反相高效液相色谱法
药动学
Andrographolide sodium bisulphite
Tetrabutyl ammonium bromide
Ion-pair extraction
Reverse-phase high performance liquid chromatographic
Pharmacokinetics
