混合分散固相萃取联合柱前衍生高效液相色谱法测定蜂蜜中草甘膦残留

Determination of glyphosate residues in honey by high performance liquid chromatography with mixed dispersion solid-phase extraction and precolumn derivatization

建立蜂蜜样品中强极性农药草甘膦的多壁碳纳米管(MWCNTs)和十八烷基硅烷键合硅胶(C18)混合分散固相萃取联合柱前试剂衍生的高效液相色谱测定方法。蜂蜜样品经水溶解后,震荡超声提取草甘膦,提取液先经60 mgMWCNTs和120mgC18混合分散固相吸附剂吸附净化,然后用1.0mg/mL9-芴基氯甲酸酯乙腈溶液进行柱前试剂衍生。目标组分经色谱柱分离后采用荧光检测器检测。草甘膦的质量浓度在0.005~5.00μg/mL范围内与色谱峰面积具有良好的线性关系,相关系数为0.9999,方法检出限为0.025 mg/kg。样品加标回收率为78.1%~92.3%,测定结果的相对标准偏差为2.8%~8.4%(n=6)。该方法可为食品卫生监管部门提供技术参考。

A high performance liquid chromatography was established for the determination of glyphosate in honey samples using multi walled carbon nanotubes(MWCNTs)and octadecylsilane bonded silica gel(C18)mixed dispersion solid-phase extraction combined with precolumn reagent derivation.After the honey sample was dissolved in water,glyphosate was extracted by shaking ultrasound.The extract was first purified by adsorption with a mixed dispersion solid-phase adsorbent of 60 mg MWCNTs and 120 mg C18,and then precolumn reagent derivatization was performed with 1.0 mg/mL 9-fluorenyl chloroformate.The target component was separated by a chromatographic column and detected using a fluorescence detector.The mass concentration of glyphosate had a good linear relationship with the chromatographic peak area in the range of 0.005-5.00μg/mL,the correlation coefficient was 0.9999,and the detection limit of the method was 0.025 mg/kg.The recovery of the sample was 78.1%-92.3%.and the relative standard deviation of the determination results was 2.8%-8.4%(n=6).This method can provide technical reference for food hygiene regulatory authorities.