[关键词]
[摘要]
目的建立小鼠血浆中杠柳毒苷的HPLC测定方法,对其药动学进行研究。方法血浆样品中加入内标地高辛,用甲醇沉淀蛋白-C18固相萃取处理,氮气吹干后流动相复溶进样。色谱条件:色谱柱为Agilent Zorbas SB-C18柱(150 mm×4.6 mm,5μm)和保护柱Agilent Zorbax C18柱(12.5 mm×4.6 mm,5μm);流动相:乙腈-水(25:75);体积流量:1.0 mL/min;柱温:25℃;检测波长:220 nm;进样量:20μL。结果此法空白血浆中无内源性物质干扰样品测定,血药浓度线性范围为0.02~2.0 mg/L(r=0.999 8),最低定量限为0.02 mg/L,平均提取回收率大于81.8%,批内、批间精密度RSD均小于4.64%,准确度试验的结果在101.3%~111.7%。结论本方法简便,准确,灵敏度高,并用于小鼠尾静脉注射杠柳毒苷的药时曲线研究。
[Key word]
[Abstract]
Objective To establish an accurate and reliable HPLC-UV method for determination of periplocin concentration in mouse plasma and apply tO pharmacokinetic studies.Methods The mouse plasma spiked with digoxin as the internal standard was deproteinized by methanol,followed by solidphase extraction with a C18 extraction cartridge,boasted the extracted solution with N2,and then redis-solve with the mobile phase.finally injeeted this solution into the HPLC instrument for determination USing a Agilent Zorbas SB-C18 column(1 50 mm×4.6 mm,5弘m)with acetonitrile-water(25:75)as mobile phase,the flow rate was 1.0 mL/min,column temperaure was 25℃,and UV detection wavelength was 220 nm.Results There was no internal substance in plasma interfered with the determination of the sampies.T‘he linear range was between 0.02-2.0 mg/L(r=0.999 8),the lower limit quantization was 0.02mg/L,the average recovery was more than 81.8%,the RSD of precision was less than 4.64%,and the accuracy was between 101.3%-111.7%.Conclusion This method iS convenient,the result iS accurate, and the sensitivity is higher.It could be successfully applied tO determination of periplocin concentration in mouse plasma during its pharmacokinetic and bioavailability studies and providing scientific basis.
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[基金项目]
天津市科技发展计划项目(05YFZJC01102);天津市高等学校科技发展基金资助项目(20050310);天津市卫生局中医、中西医结合科研基金资助项目(2005072);天津市科委应用基础研究计划项目(07JCYBJC01800)