气相色谱法检测小麦籽粒、植株及土壤中吡唑醚菌酯残留量

Determination of pyraclostrobin residues in wheat seeds, plants and soil by gas chromatography

中文关键词:  气相色谱法  固相萃取  吡唑醚菌酯  残留量  小麦

英文关键词:gas chromatography  solid-phase extraction  pyraclostrobin  residues  wheat

中文摘要:

      目的 建立固相萃取-气相色谱法测定小麦籽粒、植株和土壤中吡唑醚菌酯的残留量。方法 粉碎的小麦籽粒、植株和土壤样品经乙腈水溶液浸提, 过滤并盐析后, 分别经SPE-C18和SPE-Carb/NH2固相萃取柱净化, 采用DB-1(30 m×0.25 mm, 0.25 μm)色谱柱分离, 电子捕获检测器检测, 外标法定量。结果 吡唑醚菌酯在0.01~1.0 μg/mL线性范围内呈现良好的线性关系, 相关系数为0.9998。方法检出限为2 μg/kg。在0.01、0.10和1.0 mg/kg 3个加标水平下吡唑醚菌酯在小麦籽粒、植株和土壤中的平均回收率为79%~104%, 相对标准偏差为1.5%~5.3%。结论 该方法简便、快速、准确、重现性好, 能够有效检测小麦各组织中的吡唑醚菌酯残留量。

英文摘要:

      Objective To establish a method for the determination of pyraclostrobin residues in wheat seeds, plants and soil by solid-phase extraction-gas chromatography (SPE-GC). Methods Pyraclostrobin was extracted from crushed wheat seeds, plants and soil, soaked in acetonitrile, separated with salting out method, cleaned up with solid phase extraction column of SPE-C18 and SPE-Carb/NH2, separated by DB-1 column (30 m×0.25 mm, 0.25 μm), and detected by electron capture detector (ECD), using the external standard method for quantification. Results Pyraclostrobin had a good linear relationship in the range of 0.01~1.0 μg/mL with the correlation coefficient of 0.9998. The limit of detection was 2 μg/kg. The recoveries spiked at 3 levels of 0.01, 0.10 and 1.0 mg/kg were ranged from 79% to 104% with the relative standard deviations (RSDs) ranged from 1.5% to 5.3%. Conclusion The established method is simple, rapid, accurate and reproducible, which is suitable for the detection of pyraclostrobin in different wheat tissues.