高效液相色谱法测定水果中的灭螨醌和羟基灭螨醌

摘要

An analytical method for determination of acequinocyl and hydroxyacequinocyl in fruits was established by high performance liquid chromatography (HPLC) method. Sample was treated with hexane and ethyl acetate solution (Volume ratio was 1:1) extraction, and a Cleanert PestiCarb/NH2 SPE column was used for the purification. Then quantitative analysis was conducted by HPLC-DAD. The results showed that the mass concentration of acequinocyl and hydroxyacequinocyl behaved linearly with the area of chromatographic peak in the range of 0.01-5.0 mg/L with the correlation coefficient of 0.9999. The detection limit of acequinocyl and hydroxyacequinocyl was 0.01 mg/kg. The recovery varied from 88.5% to 102.3%, and the relative standard deviations of determination results were not more than 3.35%(n=5). The method is accurate and sensitive, and could satisfy the demand of the analysis of acequinocyl and hydroxyacequinocyl in fruits.%建立了水果中农药灭螨醌和代谢产物羟基灭螨醌的高效液相色谱测定方法.样品经过正己烷-乙酸乙酯(体积比为1:1)提取后,过石墨化碳氨基复合小柱净化,然后用高效液相色谱-荧光检测器法进行检测.结果表明,灭螨醌和羟基灭螨醌的质量浓度在0.01~5.0 mg/L范围内与色谱峰面积均呈现良好的线性关系,相关系数均为0.9999.灭螨醌和羟基灭螨醌的检出限均为0.01 mg/kg.样品加标回收率为88.5%~102.3%,测定结果的相对标准偏差不大于于3.35%(n=5).该方法灵敏度和准确度高,可满足水果中灭螨醌和羟基灭螨醌含量的测定要求.