| QuEChERS／超高效液相色谱-串联质谱法快速测定土壤中19种氟喹诺酮类抗生素残留 |
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| 基金项目:上海市科委农业领域项目(16391903800)；上海市科委技术标准专项(16DZ0501800) |
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| 中文摘要:建立了一种基于QuEChERS前处理技术，结合超高效液相色谱-串联质谱(UPLC-MS/MS)和内标法，快速测定土壤中19种氟喹诺酮类抗生素（FQs）残留的分析方法。5.0 g土壤样品添加200 μg/kg基质匹配同位素内标后，经20 mL 0.1 mol/L EDTA-McIlvaine缓冲液和乙腈混合溶剂(体积比1∶1)提取，基质分散固相萃取(150 mg无水MgSO4、15 mg PSA、15 mg C18)净化后，采用UPLC-MS/MS进行测定。质谱分析采用电喷雾电离，正离子扫描，多反应监测模式。在优化条件下，19种抗生素的相关系数(r2)为0.992~0998，检出限为0.2~1.0 μg/kg，定量下限为1.0~5.0 μg/kg；在10、50、200 μg/kg加标水平下的回收率为65.2%~104%，相对标准偏差(n=5)不大于14%。该方法操作简单快速、准确度高，适用于土壤中氟喹诺酮类抗生素残留的检测。 |
| 中文关键词:QuEChERS 超高效液相色谱-串联质谱(UPLC-MS/MS) 土壤 氟喹诺酮类抗生素（FQs） 同位素内标 基质分散固相萃取 |
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| Rapid Determination of 19 Fluoroquinolones Antibiotic Residues in Soil by QuEChERS/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract:A method of ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) combined with internal standard method was developed for the simultaneous determination of 19 kinds of fluoroquinolones antibiotic(FQs) residues in soil based on QuEChERS(Quick,Easy,Cheap,Effective,Rugged,Safe) pre-treatment.Firstly,5.0 g of soil was blended with 100 μL 10 mg/L internal standard compounds,then the analyte was extracted with 20 mL 0.1 mol/L EDTA-McIlvaine buffer and acetonitrile(1∶1,by volume),cleaned-up with a matrix dispersive solid phase extraction material(150 mg anhydrous MgSO4,15 mg PSA,15 mg C18),finally detected by UPLC-MS/MS with electrospray ionization in positive ion scanning under multiple reaction monitoring mode.Under the optimized conditions,the limits of detection and quantitation of the method were in the ranges of 0.2-1.0 μg/kg and 1.0-5.0 μg/kg,respectively,with correlation coefficients(r2) of 0.992-0998. Recoveries for 19 FQs at three spiked levels of 10,50 and 200 μg/kg ranged from 65.2% to 104% with relative standard deviations(n=5) not more than 14%.The method was simple,rapid and accurate,and was suitable for the determination of fluoroquinolones antibiotic residues in soil. |
| Key Words:QuEChERS ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) soil fluoroquinolone antibiotics(FQs) isotope labelled internal standards matrix dispersive solid phase extraction |
| 引用本文：陈磊,吴赟琦,赵志勇,赵晓燕,周昌艳.QuEChERS／超高效液相色谱-串联质谱法快速测定土壤中19种氟喹诺酮类抗生素残留[J].分析测试学报,2019,38(2):194-200. |
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