超高效液相色谱-高分辨质谱法测定蜂蜜中14种农药残留
发布时间：2019-01-04 14:50
【摘要】：目的建立超高效液相色谱-高分辨质谱同时快速测定蜂蜜中14种农药残留的方法。方法样品采用1%甲酸乙腈提取,以N-丙基乙二胺(PSA)和C18作为吸附剂的分散固相萃取法(d-SPE)进行净化,以Accucore a Q C18色谱柱(2.6μm,2.1 mm×150 mm)进行色谱分离,通过高分辨质谱的全扫描/实时二级质谱扫描模式进行定性筛查和定量检测。结果 14种农药残留在一定浓度范围内呈良好的线性关系,相关系数(r)均大于0.998,定量限(LOQ)为0.6~6μg/kg。空白蜂蜜样品在LOQ、15和30μg/kg三个加标水平的平均回收率为80.3%~112.7%,相对标准偏差为0.4%~7.1%。结论该方法适合蜂蜜中农药多残留的快速筛查和定量。
[Abstract]:Objective to establish a rapid method for the simultaneous determination of 14 pesticide residues in honey by high performance liquid chromatography-high resolution mass spectrometry. Methods the samples were extracted with 1% acetonitrile formate and purified by dispersive solid-phase extraction (d-SPE) with N-propylethylenediamine (PSA) and C18 as adsorbents, and separated by Accucore a Q C _ (18) column (2.6 渭 m ~ (2.1) mm 脳 150 mm). Qualitative screening and quantitative detection were carried out by high resolution mass spectrometry (HRMS) full scan / real-time second-stage mass spectrometry scanning mode. Results there was a good linear relationship between the 14 pesticide residues in a certain concentration range, the correlation coefficient (r) was greater than 0.998, and the quantitative limit (LOQ) was 0.6 渭 g / kg. The average recoveries of blank honey samples at LOQ,15 and 30 渭 g/kg levels were 80.3 and 112.7, and the relative standard deviation was 0.4 and 7.1. Conclusion this method is suitable for rapid screening and quantification of pesticide residues in honey.
【作者单位】： 国家食品安全风险评估中心
【基金】：国家国际科技合作专项(No.2011DFA31770)
【分类号】：R155.5
[Abstract]:Objective to establish a rapid method for the simultaneous determination of 14 pesticide residues in honey by high performance liquid chromatography-high resolution mass spectrometry. Methods the samples were extracted with 1% acetonitrile formate and purified by dispersive solid-phase extraction (d-SPE) with N-propylethylenediamine (PSA) and C18 as adsorbents, and separated by Accucore a Q C _ (18) column (2.6 渭 m ~ (2.1) mm 脳 150 mm). Qualitative screening and quantitative detection were carried out by high resolution mass spectrometry (HRMS) full scan / real-time second-stage mass spectrometry scanning mode. Results there was a good linear relationship between the 14 pesticide residues in a certain concentration range, the correlation coefficient (r) was greater than 0.998, and the quantitative limit (LOQ) was 0.6 渭 g / kg. The average recoveries of blank honey samples at LOQ,15 and 30 渭 g/kg levels were 80.3 and 112.7, and the relative standard deviation was 0.4 and 7.1. Conclusion this method is suitable for rapid screening and quantification of pesticide residues in honey.
【作者单位】： 国家食品安全风险评估中心
【基金】：国家国际科技合作专项(No.2011DFA31770)
【分类号】：R155.5
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