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

陈磊; 吴赟琦; 赵志勇; 赵晓燕; 周昌艳

doi:doi：10.3969/j.issn.1004-4957.2019.02.011

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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

更新时间：2023-04-18

- 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
- Rapid Determination of 19 Fluoroquinolones Antibiotic Residues in Soil by QuEChERS/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
- 分析测试学报 2019年38卷第2期页码：194-200
- 作者机构：
  
  1. 上海市农业科学院农产品质量标准与检测技术研究所
  2. 农业农村部农产品质量安全风险评估实验室,上海
  3. 河南农业大学食品科学技术学院
- 作者简介：
- 基金信息：
  
  上海市科委农业领域项目(16391903800);上海市科委技术标准专项(16DZ0501800)
- DOI：doi：10.3969/j.issn.1004-4957.2019.02.011
  中图分类号：
- 纸质出版：2019
- 稿件说明：
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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.

陈磊, 吴赟琦, 赵志勇, 赵晓燕, 周昌艳. Rapid Determination of 19 Fluoroquinolones Antibiotic Residues in Soil by QuEChERS/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2019, 38(2): 194-200.
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. DOI： doi：10.3969/j.issn.1004-4957.2019.02.011.

陈磊, 吴赟琦, 赵志勇, 赵晓燕, 周昌艳. Rapid Determination of 19 Fluoroquinolones Antibiotic Residues in Soil by QuEChERS/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2019, 38(2): 194-200. DOI： doi：10.3969/j.issn.1004-4957.2019.02.011.

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0.992~0998，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。

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 0.992-0998. 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.

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