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

为建立一种基于Qu ECh ERS(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、200.0μg·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2.0~5.0μg·kg~(-1),R2大于0.990。该方法可应用于农业土壤样品的检测。

Simultaneous extraction and determination of antibiotics in soils using a QuEChERS-based method and liquid chromatography-tandem mass spectrometry

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 200.0μg·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.