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

中文关键词:  高效液相色谱-串联质谱法  杀虫剂  农药残留

英文关键词:high performance liquid chromatography tandem mass spectrometry  insecticide  pesticide residues

中文摘要:

      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 C18色谱柱 (50 mm×2.1 mm, 2.6 μm, 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400 μL/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5~200 μg/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0.5~10 μg/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。

英文摘要:

      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.