气相色谱法测定小麦籽粒中吡氟酰草胺、氟噻草胺和呋草酮残留量

Determination of diflufenican, flufenacet and flurtamone residues in wheat grain by gas chromatography

中文关键词:  固相萃取  气相色谱法  吡氟酰草胺  氟噻草胺  呋草酮  农药残留  小麦

英文关键词:solid-phase extraction  gas chromatography  diflufenican  flufenacet  flurtamone  pesticide residues  wheat grain

中文摘要:

      目的 建立固相萃取-气相色谱法测定小麦籽粒中吡氟酰草胺、氟噻草胺和呋草酮3种农药的残留量。方法 粉碎的小麦籽粒样品经丙酮浸泡提取, 蒸出丙酮后用二氯甲烷萃取并浓缩, 用石油醚置换二氯甲烷后, 经Florisil-SPE小柱净化, 采用气相色谱仪HP-5(30 m×0.25 mm×0.25 μm)色谱柱分离, 电子捕获检测器检测, 以外标法定量。结果 吡氟酰草胺、氟噻草胺和呋草酮3种农药可有效分离, 线性范围分别为0.025~1.0、0.005~0.2和0.05~2.0 μg/mL, 标准曲线方程分别为Y = 22319X + 79.149, Y = 56242X ? 26.653和Y = 3285.1X ? 11.295, 相关系数均大于0.999。最低检出浓度分别为0.01、0.005、0.02 mg/kg, 平均回收率为77.0%~106.3%, 相对标准偏差2.3%~10.6%。结论 该方法简便、快速、准确、重现性好, 能够在同时检测吡氟酰草胺、氟噻草胺和呋草酮3种除草剂成分。

英文摘要:

      Objective To establish a method for the determination of diflufenican, flufenacet and flurtamone residues in wheat grain by gas chromatography. Methods Diflufenican, flufenacet and flurtamone were extracted from crushed wheat grain samples, soaked in acetone, steamed out of acetone, extracted with dichloromethane, after replacement of the petroleum ether-dichloromethane, cleaned up by florisil solid phase extraction column, separated by HP-5 column (30 m×0.25 mm, 0.25 μm) and then detected by gas chromatography equipped with electron capture detector (ECD) using the external standard method for quantification. Results Diflufenican, flufenacet and flurtamone were separated effectively in the linear ranges of 0.025~1.0, 0.005~0.2 and 0.05~2.0 μg/mL, respectively, the standard curve equations were Y = 22319X + 79.149, Y = 56242X ? 26.653 and Y = 3285.1X ? 11.295. The correlation coefficients were all over 0.999. The limits of quantification were 0.01, 0.005, 0.02 mg/kg. The recoveries were ranged from 77.0% to 106.3% with RSDs of 2.3%~10.6%. Conclusion The method is simple, rapid, and accurate, which can be used for the simultaneous detection of diflufenican, flufenacet and flurtamone in wheat grain.