建立了整体柱固相萃取-高效液相色谱/紫外检测在线联用方法并用于水果中氯吡脲的分析测定。考察了萃取溶剂的 pH 值及其流速、溶剂解吸时间及其流速等因素对氯吡脲萃取率的影响。在优化的条件下,该方法对氯吡脲的富集倍数为214倍,方法的线性范围为0.01~50.00μg / L,检出限为25 ng / L,相对标准偏差( RSD)为3.9%。黑葡萄、猕猴桃和西瓜等水果中氯吡脲的加标回收率为87.0%~120.7%,RSD 为0.6%~9.2%。结果表明该方法快速、灵敏,能满足水果中痕量氯吡脲残留分析的要求。
A novel method based on the monolithic column solid-phase extraction(SPE)cou-pled with high performance liquid chromatography in online mode was developed for the deter-mination of trace forchlorfenuron in fruits. The enrichment factor of SPE for forchlorfenuron was 214. The method was fully validated. It showed a linear range of 0. 01-50. 00 μg / L and a limit of detection of 25 ng / L,with the relative standard deviation(RSD)of 3. 9% . The proposed method was successfully applied for the determination of forchlorfenuron in grape,kiwifruit and watermelon samples,with the recoveries of 87. 0% -120. 7% and the RSDs of 0. 6% -9. 2% . This online method was proved to be selective,sensitive and convenient for the determination of trace forchlorfenuron in complex samples.
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