液相色谱-串联质谱法同时测定瓜类蔬菜及粮谷中8种农药的残留量

Simultaneous determination of 8 kinds of pesticide residues in melon vegetables and grains by liquid chromatography-tandem mass spectrography

目的建立液相色谱-串联质谱法同时检测GB 2763-2016中无推荐检测方法的8种农药(氟啶虫酰胺、氯噻啉、氟啶虫胺腈、氯虫苯甲酰胺、螺虫乙酯、丙硫克百威、氰氟虫腙、除虫菊素I)多残留检测方法。方法样品以乙腈:甲酸(99:1,V:V)作为提取剂,经QuEchERS方法前处理,采用Kinetex C_(18)色谱柱(50mm×2.1mm,2.6μm, 100?)分离,以乙腈和0.1%甲酸溶液为流动相梯度洗脱,柱温为30℃,流速为400μL/min,采用多反应监测模式检测,外标法定量。结果 8种农药在浓度为5～200μg/kg范围内线性关系良好,相关系数均大于0.99。平均加标回收率率为80.5%～109.2%,相对标准偏差为2.7%～26.3%, 8种农药的定量限为0.5～10μg/kg,符合残留分析的要求。结论该方法操作简便,适用于瓜类蔬菜及粮谷中8种农药残留量的同时测定。

Objective To establish a method for simultaneous determination of 8 kinds of pesticides （fluoroacetamides, chlorothiazoline, fluoroacetamides, chlorophenazamide, spirotetramat, propyl dithiocarbamate, cyanhydrazone, pyrethrin I） in melon vegetables and grains without recommended detection methods in GB 2763-2016 by liquid chromatography-mass spectrography. Methods Acetonitrile： formic acid （99：1, V：V） was used as the extraction agent, then the sample was pretreated by QuEchERS method, separated with a Kinetex C18 column（50 mm×2.1 mm, 2.6 μm, 100 ？） at the flow rate of 400 μL/min by gradient elution using acetonitrile and 0.1% formic acid solution. The temperature of the column was maintained at 30 ℃, the flow rate was 400 L/min. Multi-reaction monitoring mode was used to detect, and external standard method was used to quantify. Results Total of 8 kinds of pesticides had good linear relationship with the concentration of 5~200 μg/kg, and the correlation coefficients were all greater than 0.99. The average rates of recovery were 80.5%~109.2%, and the relative standard deviations were 2.7%~26.3%. The limits of quantitative of 8 kinds of pesticides were 0.5-10 μg/kg, meeting the requirements of residue analysis. Conclusion This method is easy to operate and suitable for the simultaneous determination of 8 kinds of pesticide residues in melon vegetables and grain.