改良QuEChERS/超高效液相色谱-串联质谱法同时检测蔬菜中14种喹诺酮类抗生素残留

Determination of Quinolones in Vegetables by Improved QuEChERS/Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

将QuEChERS前处理方法进行改良,以超高效液相色谱-串联质谱为检测手段,建立了同时检测蔬菜中14种喹诺酮类抗生素多残留的分析方法。样品用1.0%乙酸乙腈提取,上清液经过乙二胺-N-丙基硅烷(PSA)和无水Na2SO4净化。使用C18色谱柱分离,以乙腈-0.1%甲酸作为流动相,多反应监测模式测定,内标法定量。结果表明,14种喹诺酮类药物在1.0～100.0μg/L浓度范围内线性关系良好,三个不同添加浓度的回收率在73.8%～120%范围内,相对标准偏差在1.0%～13.5%范围内。该方法适合蔬菜中14种喹诺酮类抗生素多残留的同时检测。

The pretreatment method of QuEChERS was improved to detect the multiple residues of 14 quinolones in vegetables by ultra-high performance liquid chromatography-tandem mass spectrometer.The samples were extracted with 1.0% acetic acid-acetonitrile,and the supernatant was purified by ethylene-n-propylsilane(PSA)and anhydrous sodium sulfate.Using C18 chromatographic column separation,acetonitrile-0.1%formic acid was used as the flow phase,the multi-reaction monitoring mode was measured,and the internal standard method was used for quantification.The results showed that 14 quinolone drugs had good linear relationship within the concentration range of 1.0-100.0μg/L,and the recovery rate of three different added concentrations was within the range of 73.8%-120%,and the relative standard deviation was within the range of 1.0%-13.5%.The method can meet the requirement of quantitative analysis and simple operation,and is suitable for the detection of 14 quinolones antibiotics in vegetables.