高效液相色谱法测定儿童吡仑帕奈的血药浓度

Determination of Perampanel Concentration in Children by High Performance Liquid Chromatography

目的:建立高效液相色谱(HPLC)法检测儿童吡仑帕奈的血药浓度。方法:采用SHIMSEN ANkyLo C_(18)(4.6 mm×250 mm,5μm)色谱柱,流动相0.05%磷酸-乙腈(52∶48),柱温30℃,流速1 mL/min,进样量40μL,检测波长290 nm,检测癫痫患儿的吡仑帕奈血药浓度。结果:血清中的杂质对吡仑帕奈的检测无干扰。吡仑帕奈在80~2500μg/L线性关系良好(r=0.9998),定量限80μg/L;实测浓度在标示浓度±10%,日内/日间精密度良好(RSD均<6.0%),回收率95.73%~103.88%(RSD<2.3%);样品室温放置24 h、4℃放置7 d、-20℃放置14 d和反复冻融3次稳定性良好(RSD<3.0%)。结论:该方法检测结果准确,具有较高的灵敏度和稳定性,能满足临床对患儿吡仑帕奈血药浓度的监测及药动学研究要求。

Objective:To establish the high performance liquid chromatography(HPLC)method for the determination of pirampanel concentration in children.Methods:SHIMSEN ANkyLo C_(18)(4.6 mm×250 mm,5μm)column was adopted to separate the serum samples by a mobile phase of 0.05%phosphoric acid-acetonitrile(52∶48),the column temperature was 30℃,the flow rate was 1 ml/min,the sample volume was 40μL,and the detection wavelength was 290 nm.The concentration of perampanel in children with epilepsy was detected.Results:The impurities in serum did not interfere with the detection of perampanel.The linear range of perampanel was from 80 to 2,500μg/L(r=0.999,8),and the quantitative limit was 80μg/L.The accuracy was±10%of the marked value,and the intra-day and inter-day precision was good(RSD<6.0%),with recovery rate of 95.73%to 103.88%(RSD<2.3%).The samples stored at room temperature for 24 h,at 4℃for 7 d,at-20℃for 14 d and repeatedly frozen and thawed for 3 times had good stability(RSD<3.0%).Conclusion:The method is accurate,sensitive and stable,which can meet the clinical requirements of blood concentration and pharmacokinetic study of pirampanel in children.