超高效液相色谱-串联质谱测定酵素中14种常见杀菌剂残留
目的 建立分散固相萃取前处理技术结合超高效液相色谱-串联质谱法测定酵素中14种常见杀菌剂残留。方法 酵素样品经乙腈提取、分散固相萃取吸附剂除去色素、多糖等干扰物。采用C18色谱柱分离后, 用超高效液相色谱-串联质谱于电喷雾正离子源和多反应监测扫描模式下进行测定, 基质匹配标准曲线外标法定量。结果 14种目标化合物在20、50、100 ?g/kg 加标水平下, 回收率为81.0%~100.3%, 相对标准偏差在5.7%~12.3%之间。14种目标化合物的检出限在0.2~0.7 ?g/kg之间, 定量限在0.5~2.0 ?g/kg之间。结论 该方法前处理简单、快速, 灵敏度和准确度高, 包含种类较宽, 具有一定的拓展性, 适用于酵素中杀菌剂残留的日常监测。
Objective To establish an analytical method for determination of 14 kinds of common fungicide residues in leaven by dispersive solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Methods Leaven samples were extracted with acetonitrile, purified by dispersive solid phase extraction to remove interfering substances such as colorings and polysaccharide. The separation was performed on a C18 column, then the 14 kinds of fungicides were detected by ultra performance liquid chromatography-tandem mass spectrometry with ESI positive ion scan in mode of multiple reaction monitoring (MRM) and quantified by matrix-matched external standard method. Results At the spiked level of 20, 50 and 100 μg/kg, the recoveries of each compound were in the range of 81.0%-100.3% with the relative standard deviations of 5.7%-12.3%. The limits of detections were 0.3-0.7 μg/kg and the limits of quantitative were 0.5-2.0 μg/kg for the 14 targets compounds. Conclusion This method is simple, rapid, high sensitivity and good stability, with a wide variety and a certain development. It can be used for the daily monitoring of fungicides in leaven.
标题：超高效液相色谱-串联质谱测定酵素中14种常见杀菌剂残留
英文标题：Determination of 14 kinds of common fungicide residues in leaven by ultra performance liquid chromatography-tandem mass spectrometry
作者：
崔霞 北京市疾病预防控制中心,北京市预防医学研究中心,食物中毒诊断溯源技术北京市重点实验室
辛爽英 河北省辛集市市场监督管理局
李健潇 北京市平谷区疾病预防控制中心
周洋 北京市平谷区疾病预防控制中心
李淑云 北京市平谷区疾病预防控制中心
范赛 北京市疾病预防控制中心,北京市预防医学研究中心,食物中毒诊断溯源技术北京市重点实验室
中文关键词:分散固相萃取,超高效液相色谱-串联质谱,酵素,杀菌剂,
英文关键词:dispersive solid-phase extraction,ultra performance liquid chromatography-tandem mass spectrometry,leaven,fungicide,
发表日期：2019-02-21
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