| 王济世,贺泽英,徐亚平,王璐,彭祎,刘潇威.自动QuEChERS方法结合液相色谱串联质谱对玉米中133种农药的多残留分析[J].农业环境科学学报,2018,37(3):605-612. |
| 自动QuEChERS方法结合液相色谱串联质谱对玉米中133种农药的多残留分析 |
| Multiresidue analysis of 133 pesticides in corn using automatic QuEChERS with LC-MS/MS |
| 投稿时间：2017-08-25 |
| DOI：10.11654/jaes.2017-1166 |
| 中文关键词: 多残留分析 自动QuEChERS 玉米 液相色谱-串联质谱 |
| 英文关键词: multiresidue analysis automatic QuEChERS corn LC-MS/MS |
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| 中文摘要: |
| 基于QuEChERS（快速、简单、廉价、高效、耐用、安全）方法，借助自动QuEChERS前处理设备，结合LC-MS/MS测定手段，建立了简单、高效的同时检测玉米中133种农药多残留分析方法——自动QuEChERS。本方法将QuEChERS提取和净化两个步骤在同一设备上一次完成，操作要求低，解放了劳动力，提高了工作效率，进一步提高了实验重现性。结果表明：所有待测农药在3个添加浓度（20、100、500 μg·kg-1）的回收率在70%~120%之间（n=5），相对标准偏差小于15%。最低定量限达到2 μg·kg-1，在2~500 μg·kg-1线性范围内，相关系数大于0.99。 |
| 英文摘要: |
| In this work, a novel automatic QuEChERS methodology was developed to simplify QuEChERS procedures, while improving the sample preparation efficiency. This combination integrated QuEChERS procedures into a single run through the use of a vortex vibration-centrifuge device and a centrifuge filtration tube. To validate the efficiency of our automatic QuEChERS device, 133 pesticides in corn were analyzed using this automatic platform, combined with liquid chromatography tandem quadruple linear ion trap mass spectrometry. The results were subsequently compared with those obtained using the manual QuEChERS method. Various parameters were validated and compared, including recovery, linearity, repeatability and limits of quantification(LOQ). Satisfactory results, comparable to the results obtained using the manual QuEChERS method, were obtained. The average recoveries ranged between 70% and 120% for most pesticides, with associated relative standard deviations(RSDs) <20%(n=5), indicating satisfactory accuracy and repeatability. An LOQ of 2 μg·kg-1 was obtained for most pesticides present in the corn matrices, while the correlation coefficients were >0.990 within a linearity range of 2~500 μg·kg-1. Compared to the manual QuEChERS, this novel automatic QuEChERS device combination could significantly improve the sample preparation efficiency for the multiresidue analysis of pesticides. Actual corn samples were analyzed for method application, confirming the feasibility of the method. |
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