QuEChERS结合高效液相色谱-串联质谱法测定土壤中11类47种药物残留

Determination of 47 Drugs from 11 Categories in Soil by UPLC-MS/MS Combined with QuEChERS

摘要:

本文建立了一种QuEChERS结合高效液相色谱–串联质谱(UPLC-MS/MS)同时测定土壤中11类47种药物残留的分析方法。试验考察不同色谱柱和流动相对47种药物的分离效果，探究不同pH的EDTA-Mcllvaine缓冲液和净化填料对目标化合物的提取和净化效果，实现了对土壤中多类药物的定量分析。47种药物在对应线性范围内均呈现较好的线性关系(r≥0.995)；方法的检出限为0.1 ~ 2.5 μg/kg，定量限为0.5 ~ 8 μg/kg；3水平加标试验的回收率为61.1% ~ 117.0%，相对标准偏差为1.9% ~ 11.4%。该方法适用于土壤多组分准确高通量定量分析，检出限、回收率、准确度均符合分析要求，为土壤中多种药物的赋存底数和潜在风险研究提供技术支撑。

Abstract:

In this study, a UPLC-MS/MS method combined with QuEChERS was established to simultaneously determine 47 drugs from 11 categories in soil, separation effects of different columns and mobile phases on the analytes were addressed, and extraction effects of EDTA-Mcllvaine buffer solution with different pH and purification effects of d-SPE dispersers on drugs were also analyzed. The results showed that all the 47 drugs showed good linearity with r≥0.995, LODs of 47 compounds ranged from 0.1 to 2.5 μg/kg, LOQs ranged from 0.5 to 8 μg/kg, recoveries varied between 61.1% and 117.0%, and RSDs from 1.9% to 11.4%. This UPLC-MS/MS method is sensitive and suitable for accurate and high throughput analysis of multiclass drugs residues in soil. Thus, it is useful for analysis of occurrence characteristics and risk assessment of drugs residues in soil.