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
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。
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.
标题：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
英文标题：Determination of pyraclostrobin residues in wheat seeds, plants and soil by gas chromatography
作者：
杨茜茹 河北省农林科学院农产品质量安全研究中心,农业部农产品质量安全风险评估实验室(石家庄)
范立欣 河北省农林科学院农产品质量安全研究中心,农业部农产品质量安全风险评估实验室(石家庄)
钱训 河北省农林科学院农产品质量安全研究中心,农业部农产品质量安全风险评估实验室(石家庄)
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,
发表日期：2017-02-09
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