固相萃取-HPLC法测定浓缩梨汁中噻菌灵、多菌灵的残留量
Simultaneous Determination of Thiabendazole and Carbendazim Residues in Concentrated Pear Juice by Solid Phase Extraction-HPLC
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摘要: 研究了一种可同时测定浓缩梨汁中噻菌灵和多菌灵残留量的固相萃取-高效液相色谱分析方法.浓缩梨汁样品与水按一定比例稀释后,经过调pH、离心、过滤,用混合相固相萃取小柱(Mixed-mode SPE)进行提取、净化,用配有二级管阵列检测器(DAD)的液相色谱仪检测,外标法定量.使用噻菌灵和多菌灵对照品进行添加回收率测定,结果显示本方法对噻菌灵的最低检出限为0.020 mg/kg,回收率为80.5%~84.3%;对多菌灵的最低检出限为0.020 mg/kg,回收率为83.2%~92.5%;测定的相对标准偏差均不大于5%.本方法简单、快速、准确,能满足常规噻菌灵和多菌灵残留量检测的需要.Abstract: A solid phase extraction-high performance liquid chromatographic(HPLC) method was developed for the simultaneous analysis of thiabendazole and carbendazim in concentrated pear juice.The sample was previously diluted with distilled water.After centrifuging,filtering and adjusting the pH,the sample was extracted and cleaned up with Mixed-mode SPE,and determinated the quantities of thiabendazole and carbendazim residues by HPLC with DAD using external standard method.The detection limit was 0.020 mg/kg for both.The recovery was 80.5%~84.3% for thiabendazole and 83.2%~92.5% for carbendazim,and the relative standard deviation(RSDs) was all no more than 5%.The method is simple,fast and sufficient for routine analysis.