大米中193种农药多残留检测方法的研究

Detection Methods of 193 Multi-pesticide Residues in Rice

由于大米农残检测需求及检测项目的不断扩增,建立高效、可靠的多农残分析方法具有重要意义。为了建立一种全自动在线定量浓缩净化色谱（GPC）-液相色谱-三重四级杆线性离子阱质谱（LC-Q-TRAP/MS）法测定大米中193种农药残留量,将大米样品经乙腈超声提取,GPC全自动在线定量浓缩净化,由三重四级杆线性离子阱质谱仪定性及定量检测。试验结果表明：方法的线性关系良好,相关系数R均大于0.9904,检出限（LOD）为5μg·kg^-1,定量限（LOQ）为10μg·kg^-1;193种农药在添加水平为5μg·kg^-1时的平均回收率范围为66.2%～124.3%,相对标准偏差（RSD）范围为3.4%～17.8%;在添加水平为10μg·kg^-1时的平均回收率范围为69.4%～115.7%,相对标准偏差（RSD）范围为2.9%～16.3%。该方法具有较高的灵敏度和准确度,并且自动化程度较高,能满足国内外对大米农药残留检测要求。

For the increasing need of rice detection and test items, establishment of high automatic testing method is very important. We presented a detection method for the simultaneous determination of 193 pesticide residues in rice by gel permeation chromatography（GPC）- liquid chromatography-triple quadrupole-linear ion trap mass spectrometry（LC-Q-TRAP/MS）. Rice samples were ultrasonically extracted with acetonitrile, and automatically line quantitative concentrated and purified by GPC, and qualitatively and quantitatively detected by LC-Q-TRAP/MS. The testing results showed that the good linear was obtained with correlation coefficients more than0.9904, the limit of detection（LOD） was 5μg·kg^-1and the limits of quantity（LOQ） was 10 μg·kg^-1. At spiked level of 5μg·kg^-1, the average recoveries of 193 pesticides in rice range from 66.2% to 124.3% with relative standard deviation（RSD） was between 3.4% and17.8%. At spiked level of 10 μg·kg^-1, the average recoveries of 193 pesticides in rice ranged from 69.4% to 115.7% with relative standard deviation（RSD） between 2.9% and 16.3%. This method is effective, sensitive and highly efficient in pretreatment to the determination of pesticide residues in rice.