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    分散固相萃取-液质联用法测定烟叶中氟吡甲禾灵及代谢物

    Determination of Haloxyfop-methyl and Its Metabolites in Tobacco by Dispersive Solid-Phase Extraction Coupled with Liquid Chromatography-Mass Spectrometry

    • 摘要: 建立了分散固相萃取-高效液相色谱-串联质谱法(HPLC-MS/MS)测定烟叶中氟吡甲禾灵及其代谢物氟吡禾灵。在碱性条件下(pH≥10),样品中的氟吡甲禾灵及其共轭物全部水解为氟吡禾灵,经乙腈提取,分散固相萃取净化,HPLC-MS-MS检测。氟吡甲禾灵在鲜烟叶中的添加水平为0.02~1.0 mg/kg时,平均回收率为93%~99%,相对标准偏差为3.1%~4.9%;在干烟叶中的添加水平为0.05~1.0 mg/kg时,平均回收率为92%~96%,相对标准偏差为3.3%~4.6%。氟吡禾灵鲜烟叶和干烟叶的标准曲线在0.005~1.0 mg/kg范围内线性关系良好,相关系数均大于0.99。氟吡甲禾灵在鲜烟叶和干烟叶中的定量限分别为0.02和0.05 mg/kg,实际检测样品氟吡甲禾灵在鲜烟叶和干烟叶中的残留量均小于其定量限。该方法简便、可靠、高效、快捷,适用于烟叶样品中氟吡甲禾灵及其代谢物氟吡禾灵的残留检测。

       

      Abstract: A method was developed for determination of haloxyfop-methyl and its metabolite haloxyfop in tobacco leaves using dispersive solid phase extraction-high performance liquid chromatography-tandem triple quadrupole mass spectrometry (HPLC-MS/MS). Under alkaline condition (pH≥10), haloxyfop-methyl and its conjugate in samples were hydrolyzed to haloxyfop. The samples were extracted by acetonitrile, purified by dispersive solid phase extraction, and detected by HPLC-MS/MS. The average recoveries were 93%-99% and the relative standard deviations (RSDs) were 3.1%-4.9% when haloxyfop-methyl was added at 0.02-1.0 mg/kg in fresh tobacco leaves. The average recoveries were 92%-96% and the RSDs were 3.3%-4.6% when haloxyfop-methyl was added at 0.05-1.0 mg/kg in dry tobacco leaves. The linear relationships between the standard curves of fresh and dry tobacco leaves were good in the range of 0.005-1.0 mg/kg, and the correlation coefficients were all greater than 0.99. The limit of quantitations (LOQs) of haloxyfop-methyl in fresh tobacco leaves and dry tobacco leaves were 0.02 mg/kg and 0.05 mg/kg, respectively. The residue of haloxyfop-methyl in both fresh and dry tobacco leaves were lower than its LOQs. This method is simple, reliable, efficient, and rapid, and is suitable for the determination of haloxyfop-methyl and its metabolite haloxyfop residues in tobacco samples.

       

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