超高效液相色谱-串联质谱法快速检测海南特色“土壤-蔬菜”系统复杂混合基质中恩诺沙星残留

Rapid detection of enrofloxacin residues in complex mixed matrix of Hainan’s special “soil-vegetable” system by ultra performance liquid chromatography-tandem mass spectrometry

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  ultra performance liquid chromatography-tandem mass spectrometry  “soil-vegetable” system  complex mixed matrix  antibiotic residues  antibiotic resistance genes

中文摘要:

      目的 建立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%乙二胺四乙酸(ethylene diamine tetraacetic acid, EDTA)-Mcllvaine缓冲溶液]涡旋超声提取, 离心沉降, 溶剂转换, 0.22 μm尼龙滤膜过滤后, 以乙腈和0.1%甲酸水溶液(含2 mmol/L乙酸铵)为流动相, 经Waters ACQUITY UPLC? BEH C18色谱柱(2.1 mm×100 mm, 1.7 μm)梯度洗脱分离, 使用质谱仪作为检测器对恩诺沙星进行定性定量。结果 在1~200 ng/mL的质量浓度范围中, 标准曲线线性关系良好(相关系数为0.9996), 方法的检出限为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:

      Objective To establish an analytical method for the determination of enrofloxacin residues in complex mixed matrix of the “soil-vegetable” system by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was subjected to vortex ultrasonic extraction with acidified acetonitrile extract [containing 5% ethylene diamine tetraacetic acid (EDTA)-Mcllvaine buffer solution], settling with centrifugation, getting solvent conversion and being filtered by 0.22 μm nylon filter membrane. The mobile phase was composed of acetonitrile and 0.1% formic acid aqueous solution (containing 2 mmol/L ammonium acetate), and the mixture was subjected to Waters ACQUITY UPLC ? BEH C18 chromatographic column (2.1 mm×100 mm, 1.7 μm) gradient elution separation, using mass spectrometry as a detector for qualitative and quantitative analysis of enrofloxacin. Results In the mass concentration range of 1–200 ng/mL, the standard curve showed a good linear relationship (correlation coefficient=0.9996), the limit of detection of the method was 0.11 μg/kg, the recovery rates 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.