摘要
[目的]建立超高效液相色谱-串联质谱法同时测定粮谷中18种农药残留检测方法。[方法]采用超高效液相色谱-串联质谱法;乙腈提取后中性氧化铝柱净化;C_(18)柱分离,流动相0.1%甲酸-乙腈梯度洗脱,柱温35℃,进样量10μL;电喷雾正离子模式,毛细管电压3.50 kV,源温度120℃,脱溶剂气温度400℃,脱溶剂气流量700 L/h,碰撞室压力2.7×10~(-3) mbar。[结果]18种农药残留在各自检测浓度性范围内线性关系良好,其中11种农药R~2>0.999,其他R~2>0.99;检测限和定量限均低于国家标准;13种农药平均加标回收率均为80%~104%,仅5种平均加标回收率为62%~84%。
[Aims] A method for simultaneous determination of 18 pesticide residues in cereal grains by ultra high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) was developed. [Methods] The determination was conducted by ultra high performance liquid chromatography tandem mass spectrometry, the samples were extracted with acetonitrile, purified with neutral alumina column, separated by C_(18) column with gradient elution of the mixture of 0.1% formic acid and acetonitrile, column temperature was 35 ℃, and injection volume was 10 μL. The conditions were: electrospray positive ion mode, capillary voltage 3.50 k V, source temperature 120 ℃, desolvation gas temperature 400 ℃, desolvation gas flow 700 L/h, collision chamber pressure of 2.7×10~(-3) mbar. [Results] The 18 kinds of pesticide residues have good linear relation in the range of their detection concentration, 11 pesticide residues were R~2>0.999 and the remaining R~2>0.99; the average recovery rate of the 13 pesticides were 80-104%, and average recovery rates of 5 kinds were 62-84%.
引文
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