超高效液相色谱-串联质谱法测定粮谷中18种农药残留

Determination of 18 Pesticide Residues in Cereals by UPLC-MS/MS

[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 C18 column with gradient elution of the mixture of 0.1% formic acid and acetonitrile, column temperature was 35℃, and injection volume was 10μL. The conditions were： eleetrospray positive ion mode, capillary voltage 3.50 kV, 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 R2〉0.99; the average recovery rate of the 13 pesticides were 80-104%, and average recovery rates of 5 kinds were 62-84%.