气相色谱-串联质谱法检测大米中20种农药残留

发布时间：2018-08-25 07:12

【摘要】：建立了两种可简便、灵敏、快速、批量测定大米中20种农药残留的分析方法。样品经乙腈提取后,使用C18固相萃取柱(SPE)和Qu ECh ERS两种不同净化方法,采用气相色谱-串联质谱选择反应监测(SRM)模式对20种农药进行检测,通过保留时间、选择离子及其相对丰度定性,外标法定量。结果表明,20种农药的线性范围为0.01~0.2μg/m L,相关系数均大于0.99。在0.01,0.05,0.20 mg/kg加标水平下,采用C18柱对大米样品进行提取净化,20种农药的平均回收率为63.3%~96.0%,相对标准偏差(RSD)为1.9%~13.9%;采用Qu ECh ERS方法对大米样品进行提取净化,20种农药的平均回收率为67.7%~121.0%,RSD为1.9%~16.4%。此两种方法无明显差异,为农药多残留检测提供了不同的思路,能够对大批量大米样品进行同时检测,数据准确可靠,回收率与精密度均符合农药残留的分析要求。
[Abstract]:Two simple, sensitive, rapid and batch analytical methods for the determination of 20 pesticide residues in rice were established. After being extracted by acetonitrile, 20 pesticides were detected by gas chromatography-tandem mass spectrometry (GC-MS) selective reaction monitoring (SRM) mode using C18 solid-phase extraction column (SPE) and Qu ECh ERS purification methods. Select ions and their relative abundance qualitative, quantitative external standard method. The results showed that the linear range of 20 pesticides was 0. 01 ~ 0. 2 渭 g / mL, and the correlation coefficients were all greater than 0. 99. The average recoveries of 20 pesticides extracted and purified by C18 column were 63.3% and 96.0, and the relative standard deviation (RSD) was 1.90.The average recovery of 20 pesticides extracted and purified by Qu ECh ERS was 67.7121.0% and 1.97.121.0%, respectively, and the average recovery of 20 pesticides was 1.97.121.00.The average recoveries of 20 pesticides in rice samples were 67.7121.0% and 1.916.4% respectively, and the relative standard deviation (RSD) was 1.90.0.The average recovery of 20 pesticides in rice samples was 67.7121.00.The average recoveries of 20 pesticides were 67.7121.0%. There was no obvious difference between the two methods, which provided different ideas for the multi-residue detection of pesticides, and could be used for simultaneous detection of large quantities of rice samples. The data were accurate and reliable, and the recovery and precision were in line with the requirements of pesticide residue analysis.
【作者单位】：沈阳农业大学植物保护学院;大连出入境检验检疫局检验检疫技术中心;辽宁出入境检验检疫局检验检疫技术中心;
【基金】：国家质检总局科研项目(2010IK134)
【分类号】：O657.63;TS210.7

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