液相色谱-串联质谱法测定果蔬酱中13种吡啶和嘧啶类除草剂

Determination of 13 pyridine and pyrimidine herbicides in fruit and vegetable sauce by liquid chromatography-tandem mass spectrometry

目的建立果蔬酱中13种吡啶和嘧啶类除草剂的多残留液相色谱-串联质谱方法。方法样品经乙腈(含1%甲酸)提取、QuEChERS(quick,easy,cheap,effective,rugged and safe)技术净化后用ZORBAX SB-Aq柱(2.1 mm×150 mm,3.5μm)分离,以乙腈-0.1%甲酸水溶液(含5 mmol/L乙酸铵)为流动相进行梯度洗脱,以液相色谱-串联质谱法(liquid chromatographytandem mass spectrometric,LC-MS/MS)的多反应监测模式(multi-reaction monitoring,MRM)检测,外标法定量。结果13种吡啶和嘧啶类除草剂在各自的浓度范围内线性关系良好,相关系数(r)均>0.999,3个不同浓度的平均加标回收率为80.36%~118.74%,相对标准偏差为0.22%~9.62%,方法检出限为0.06~1.60μg/kg。结论该方法操作简单、灵敏度高、重复性好,可用于果蔬酱中13种吡啶和嘧啶类除草剂的同时检测。

Objective To establish a multi residue liquid chromatography-tandem mass spectrometric(LC-MS/MS)method for the determination of 13 pyridine and pyrimidine herbicides in fruit and vegetable sauce.Methods The samples were extracted with acetonitrile(containing 1%formic acid),purified using QuEChERS(quick,easy,cheap,effective,rugged and safe)technology,and separated using a ZORBAX SB-Aq column(2.1 mm×150 mm,3.5μm).The gradient elution was performed using an acetonitrile 0.1%formic acid aqueous solution(containing 5 mmol/L ammonium acetate)as the mobile phase,and detected using LC-MS/MS in multiple-reaction monitoring(MRM)mode.Quantification was performed using an external standard method.Results 13 pyridine and pyrimidine herbicides showed good linear relationships within their respective concentration ranges,with correlation coefficients greater than 0.999.The average recovery rates for three different concentrations ranged from 80.36%to 118.74%,with relative standard deviations of 0.22%to 9.62%,and the limits of detection was 0.06-1.60μg/kg.Conclusion The method is simple and sensitive,with good reproducibility,and can be used for simultaneous detection of 13 pyridine and pyrimidine herbicides in fruit and vegetable sauce.