论文部分内容阅读
目的建立液相色谱-串联质谱法同时检测毛豆中21种常用农药残留的分析方法。方法样品以乙腈-甲酸(99:1,V:V)作为提取剂,经Qu ECh ERS方法前处理,采用Phenomenex的Kinetex C_(18)色谱柱(50 mm×2.1mm,2.6μm,100?)分离,以乙腈-0.1%甲酸水溶液为流动相梯度洗脱,以电喷雾电离(ESI)、正离子模式和负离子模式2种多反应监测(MRM)模式检测,外标法定量。结果 21种农药在5~200 ng/m L范围内,线性相关系数均大于0.99,线性良好。分析目标物添加水平为0.01~0.10 mg/kg时,回收率范围为73%~113%,RSD范围为1.3%~10.9%,符合残留分析的要求。21种农药的定量下限为0.01 mg/kg。结论该方法的提取简便,基质分散效果好,灵敏度满足国内外限量标准的要求,适合毛豆中常用农药残留的同时测定。
Objective To establish a method for the simultaneous determination of 21 common pesticide residues in Glycine max by liquid chromatography - tandem mass spectrometry. Methods The samples were separated on a Kinetex C 18 column (50 mm × 2.1 mm, 2.6 μm, 100 μm) on a Phenomenex column with acetonitrile-formic acid (99: 1, V: V) The fractions were separated and eluted with a mobile phase of acetonitrile-0.1% formic acid. The mobile phase was eluted with electrospray ionization (ESI), positive ion mode and negative ion mode (MRM). Results The linear correlation coefficient of 21 kinds of pesticides in the range of 5 ~ 200 ng / m L were all above 0.99 with good linearity. The recoveries ranged from 73% to 113% and RSD ranged from 1.3% to 10.9% at the target level of 0.01-0.10 mg / kg, which met the requirements of residue analysis. The lower limit of quantitation for 21 pesticides is 0.01 mg / kg. Conclusion The extraction method is simple, the matrix dispersion effect is good, and the sensitivity meets the requirements of domestic and international limit standards. It is suitable for the simultaneous determination of common pesticide residues in soybean.