| 孟明辉,贺泽英,徐亚平,王璐,彭祎,刘潇威.QuEChERS方法结合高效液相色谱-串联质谱法同时测定土壤中20种抗生素[J].农业环境科学学报,2017,36(8):1672-1679. |
| QuEChERS方法结合高效液相色谱-串联质谱法同时测定土壤中20种抗生素 |
| Simultaneous extraction and determination of antibiotics in soils using a QuEChERS-based method and liquid chromatography-tandem mass spectrometry |
| 投稿时间：2017-03-01 |
| DOI：10.11654/jaes.2017-0249 |
| 中文关键词: QuEChERS 抗生素 多残留分析 土壤 液相色谱-串联质谱 |
| 英文关键词: QuEChERS antibiotics multi-residue analysis soil LC-MS/MS |
| 基金项目:中国农业科学院创新工程项目 |
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| 中文摘要: |
| 为建立一种基于QuEChERS（快速Quick、简单Easy、廉价Cheap、高效Effective、耐用Rugged、安全Safe）同时测定土壤中20种抗生素多残留的分析方法，土样经提取液（EDTA，乙腈：磷酸盐）提取、分散固相萃取材料（PSA，C18）净化后，采用液相色谱串联质谱（LC-MS/MS）进行测定。通过试验优化了不同提取方法、净化吸附剂比。结果表明：该方法在7个添加水平（2.0、5.0、10.0、20.0、50.0、100.0、200.0 μg·kg-1）下具有良好的回收率，回收率范围为61.4%~118.9%，相对标准偏差小于20%（n=5）；绝大多数抗生素的方法定量限为2.0~5.0 μg·kg-1，R2大于0.990。该方法可应用于农业土壤样品的检测。 |
| 英文摘要: |
| The aim of this work was to develop a method, based on QuEChERS(quick, easy, cheap, effective, rugged, and safe), to extract and analyze residues of 20 antibiotics in soil. The developed method included extraction with an ACN:EDTA:McIlvaine buffer, clean-up with a dispersive solid phase extraction(d-SPE) adsorbent using primary secondary amine(PSA) and octadecylsilane(C18), and finally analyte determination using liquid chromatography-tandem mass spectrometry(LC-MS/MS). This work optimized different extraction methods and ratios of clean-up adsorbents to perform at seven spiking levels(2.0, 5.0, 10.0, 20.0, 50.0, 100.0, and 200.0 μg·kg-1) with recoveries ranging from 61.4% to 118.9% with relative standard deviations below 20%(n=5). The limits of quantification(LOQ) of the methods were in the range of 2.0~5.0 μg·kg-1 for most analytes. Linear regression coefficients of greater than 0.990 were obtained. This method was applied to the analysis of real agricultural soil samples, confirming the feasibility of the method. |
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