SPE-HPLC法分析大鼠血浆中灭多威

摘要

目的 建立以同相萃取-高效液相色谱(SPE-HPLC)分析大鼠血浆中灭多威的方法.方法 以空白大鼠血浆添加灭多威标准品及内标物,以SPE法对样品进行前处理,采用HPLC进行分析,考察仪器测试条件、特异性、回收率、灵敏度、精密度、准确度、线性关系、稳定性,并对方法进行优化.结果 采用本文方法测得灭多威在血浆中的线性范围0.1-20μg/mL(r=0.9993,P<0.001),血浆中的检测限0.03μg/mL(S/N≥3),日内、日间精密度的CV值分别在8.33%与11.11%以内,日内、日间准确度值分别在90%与120%之间,回收率值在88%±4.4%以上.结论 所建方法实用、便捷,可对血浆中的灭多威进行定性定量地快速测定.%Objective To establish a method of solid phase extraction-reversed-phase high performance liquid chromatography(SPE-HPLC)for determination of methomyl in plasma of rat.Methods The sample pretreatment method,the test conditions,the linear range,the sensitivity,the specificity,the precision, the accuracy,the stability and the recoveries for plasma were investigated by using rat plasma spiked with standard methomyl and intemal standard substance.Results The linear range was 0.1～20μg/mL ( r= 0.9993,P<0.001).The limit of detection was 0.03μg/mL(S/N ≥3).The intra and inter-day precision of assay for methomyl was less than 8.33%and 11.11%in plasma respectively.The intra and inter-day accuracy of assay for methomyl was between 90%and 120%in plasma respectively.The recoveries for methomyl were more than 88%±4.4%in plasma.Conclusion The HPLC method for quantitative and qualitative analysis of methomyl is simple,rapid and accurate,which is suitable for the identification of methomyl in the cases.