QuEChERS-液质联用法测定菜籽油中7种芳氧苯氧丙酸酯类除草剂残留

Determination of seven aryloxyphenoxypropionate herbicides residues in rapeseed oil by QuEChERS-liquid chromatography/tandem mass spectrometry

建立了分散固相萃取(QuEChERS)净化方法结合液质联用(HPLC-MS/MS)检测技术同时测定菜籽油中7种芳氧苯氧丙酸酯类除草剂的方法。结果表明:最优检测条件为采用90%乙腈水溶液提取2次,Supel QuE Z-Sep+分散固相萃取净化,色谱柱为sunshell C18柱(2.6μm×2.1 mm×100 mm),以乙腈和0.025%乙酸水溶液进行梯度洗脱,MRM模式。在最优检测条件下,除精恶唑禾草灵外6种除草剂线性范围0~100(50)μg/L,相关系数R大于0.999 5,定量限在0.25~2.5μg/kg之间,回收率在78.3%~95.1%之间,相对标准偏差在0.9%~6.5%之间。方法具有基质效应低、处理简单、准确快速、重复性好的优点,适用于实验室高通量快速检测菜籽油样品。

A QuEChERS - liquid chromatography/tandem mass spectrometry to determine seven aryloxy- phenoxypropionate herbicides in rapeseed oil was developed. The results showed that the optimal detec- tion conditions were obtained as follows：samples extracted by 90% acetonitrile water solution for twice, extractive purified by Supel QuE Z -Sep and dispersive solid -phase extraetion, ehromatography eolumn sunshell C18（2.6μm×2. 1 mm×100 mm） ; mobile phase acetonitrile and 0. 025% acetic acid water solution, gradient elution, MRM method. Under the optimal detection conditions, except for fenoxaprop -ethyl, the calibration curve was linear in the range of 0 -100（50）μg/L and R 〉 0. 999 5, and the limit of quanti- tation was in the range of 0.25 - 2.5 μg/kg. The recovery rate and relative standard deviation were in the range of 78.3% -95.1% and 0.9% -6.5%, respectively. The method had advantages of low ma- trix effect, easy sample handling, accuracy, rapidness, and good reproducibility, and could be used as a high throughput and rapid detection method for rapeseed oil in lab.