摘要
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.
作者
刘畅
LIU Chang(Harbin Examing and Inspection Center for Agricultural Products Safety and Quality,Harbin 150000)
出处
《分析科学学报》
CAS
CSCD
北大核心
2019年第1期124-128,共5页
Journal of Analytical Science
关键词
QUECHERS
超高效液相色谱-串联质谱
蔬菜
喹诺酮
多残留
QuEChERS
Ultra-high performance liquid chromatography-tandem mass spectrometry
Vegetables
Quinolone
Residuals