高效液相色谱-串联质谱法检测玉米中磺草酮残留

Determination of sulfonate residues in corn by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  磺草酮  玉米  高效液相色谱-串联质谱法  固相萃取  微孔滤膜

英文关键词:sulfoketone  corn  high performance liquid chromatography-tandem mass spectrometry  solid phase extraction  millipore filter

中文摘要:

      目的 建立高效液相色谱-串联质谱法检测玉米中磺草酮残留的分析方法。方法 样品用乙腈超声提取 20 min, 经石墨化碳固相萃取柱净化, 用乙腈+甲苯(3:1, V:V)洗脱, 洗脱液于35 ℃水浴浓缩, 用20% (V:V)甲醇水溶液(含0.1%甲酸)溶解定容, 过0.22 μm亲水聚四氟乙烯(polytetrafluoroethylene, PTFE)微孔滤膜, 采用高效液相色谱-串联质谱仪进行检测。结果 磺草酮在1~200 μg/L质量浓度范围内线性关系良好, 相关系数为0.9998; 检出限为2 μg/kg, 定量限为10 μg/kg; 添加水平为0.01~0.05 mg/kg时, 回收率范围为80.3%~108.6%, 相对标准偏差为2.4%~4.4%。结论 该检测方法快速、简便, 准确度和精密度均能满足日常监测的需求, 能满足玉米中磺草酮批量检测的需要。

英文摘要:

      Objective To establish a method for the determination of sulfodone residues in corn by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were ultrasonically extracted with acetonitrile for 20 min, purified by a graphitized carbon solid phase extraction column, and eluted with acetonitrile+toluene (3:1, V:V), the eluent was concentrated in 35 ℃ water bath, dissolved and fixed to constant volume by 20% (V:V) methanol aqueous solution (containing 0.1% formic acid), filtered by 0.22 μm hydrophilic polytetrafluoroethylene (PTFE) microporous filter membrane and detected by high performance liquid chromatography- tandem mass spectrometer. Results Sulcotrione had a good linear relationship in the mass concentration range of 1?200 μg/L, wiht the correlation coefficient 0.9998. The limit of detection was 2 μg/kg, and the limit of quantification was 10 μg/kg; when the addition level was 0.01?0.05 mg/kg, the recoveries ranged from 80.3% to 108.6%, and the relative standard deviations were 2.4% to 4.4%. Conclusion This method is rapid, simple, accurate and precise to meet the needs of daily monitoring, which can meet the needs of batch detection of sulfoketone in corn.