QuEChERS/高效液相色谱-串联质谱法测定土壤中61种激素类药物残留

Determination of 61 Hormone Residues in Soil by QuEChERS/High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了QuEChERS/高效液相色谱-串联质谱(HPLC-MS/MS)测定土壤中61种激素类药物残留的分析方法。样品经乙腈提取,QuEChERS方法净化后进行HPLC-MS/MS测定。采用电喷雾离子源(ESI),正、负模式扫描,多反应监测(MRM)模式采集,基质匹配工作曲线法定量。结果表明:61种目标化合物在各自浓度范围内线性良好,相关系数(r^2)为0.991 8~0.999 8,检出限(LOD,S/N≥3)为0.01~2.3μg/kg,定量下限(LOQ,S/N≥10)为0.03~7.5μg/kg;在10、50、200μg/kg 3个加标水平下,平均回收率为62.6%~102%,相对标准偏差(n=6)为1.0%~11%。该方法简单、快速、重现性好、稳定性高,可满足土壤中61种激素类药物残留的检测要求。

A QuEChERS/high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS)method was developed for the determination of 61 kinds of hormone residues in soil.Samples were extracted with acetonitrile,and then purified using QuEChERS method.Analysis on the targets was performed by electrospray ionization mass spectrometry in positive or negative mode,multiple reaction monitoring(MRM)mode was used for collection,and matrix matched standard curve method was selected for quantitation.Results showed that 61 analytes showed good linearities in their respective ranges,with correlation coefficients(r 2)between 0.991 8 and 0.999 8.The limits of detection(LOD,S/N≥3)were 0.01-2.3μg/kg while the limits of quantitation(LOQ,S/N≥10)were 0.03-7.5μg/kg.Recoveries for the target analytes at spiked levels of 10,50 and 200μg/kg ranged from 62.6%to 102%,with relative standard deviations(n=6)of 1.0%-11%.The method is simple,rapid,replicable and high stable,and could meet the requirements for determination of 61 hormone residues in soil.