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| 建立快速检测海南特色“土壤-蔬菜”系统复杂混合基质中恩诺沙星残留的分析方法 |
| Rapid detection of Enrofloxacin residues in complex mixed matrix of Hainan"s special |
| 投稿时间：2025-02-19 修订日期：2025-06-09 |
| DOI： |
| 中文关键词: 恩诺沙星 超高效液相色谱－串联质谱法 “土壤－蔬菜”系统 复杂混合基质 抗生素残留 抗生素耐药性基因 |
| 英文关键词:Enrofloxacin UPLC-MS/MS Soil-vegetable system complex mixed matrix Antibiotic residues ARGs |
| 基金项目:国家市场监督管理总局重点实验室(热带果蔬质量与安全)自主研究课题项目(ZZ-2024007)资助 |
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| 中文摘要: |
| 目的? 本文建立了一种基于超高效液相色谱－串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定海南特色“土壤－蔬菜”系统中复杂混合基质恩诺沙星残留的分析方法。方法? 样品经酸化乙腈提取液（含5%EDTA-Mcllvaine缓冲溶液）涡旋超声提取，离心沉降，溶剂转换，0.22μm尼龙滤膜纯化后，以乙腈和0.1%甲酸水溶液（含2mmol/L乙酸铵）为流动相，经Waters ACQUITY UPLC? BEH C18色谱柱( 1.7μm 2.1*100mm)梯度洗脱分离，使用质谱作为检测器对恩诺沙星进行定性定量。结果? 在 1~ 200ng/mL 的浓度范围中，标准曲线线性关系良好（相关系数 = 0.9996），方法的检测限为 0.11 μg/kg，加标回收率范围为87.4%~103.3%，相对标准偏差(relative standard deviations, RSDs)为 0.4%~4.0%(n=6)。结论? 该分析方法快速、准确、重复性良好，适用于“土壤－蔬菜”系统复杂混合基质中恩诺沙星残留的检测，拥有间接揭示系统中抗生素耐药性基因(antibiotic resistance genes, ARGs)污染风险的潜力。 |
| 英文摘要: |
| ABSTRACT:Objective? This article established an analytical method for the determination of enrofloxacin residues in complex mixed matrix of the "soil-vegetable" system using UPLC-MS/MS(ultra performance liquid chromatography tandem mass spectrometry). Methods? The sample was subjected to vortex ultrasonic extraction with acidified acetonitrile extract (containing 5% EDTA Mcllvaine buffer solution), settling with centrifugation,getting solvent conversion and being purified by 0.22 μm nylon filter membrane. The mobile phase was composed of acetonitrile and 0.1% formic acid aqueous solution (containing 2mmol/L ammonium acetate), and the mixture was subjected to Waters ACQUITY UPLC ? BEH C18 Chromatographic column (1.7 μm 2.1 * 100mm) gradient elution separation, using mass spectrometry as a detector for qualitative and quantitative analysis of enrofloxacin. Results In the concentration range of 1-200ng/mL, the standard curve showed a good linear relationship (correlation coefficient=0.9996), the detection limit of the method was 0.11 μg/kg, the recovery rate ranged from 87.4% to 103.3%, and the relative standard deviations (RSDs) were 0.4% to 4.0% (n=6). Conclusion? This method has fast analysis speed, high accuracy, and good repeatability, and is suitable for the detection of enrofloxacin residues in complex mixed matrix of the "soil-vegetable" system.It also has the potential to indirectly reveal the risk of antibiotic resistance genes (ARGs) contamination in the system. |
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