徐永, 寿林飞, 虞淼, 徐正宁. 超高效液相色谱-串联四级杆质谱联用法测定水果中多效唑、氯吡脲和咪鲜胺的残留[J]. 农药学学报, 2012, 14(1): 61-66.
    引用本文: 徐永, 寿林飞, 虞淼, 徐正宁. 超高效液相色谱-串联四级杆质谱联用法测定水果中多效唑、氯吡脲和咪鲜胺的残留[J]. 农药学学报, 2012, 14(1): 61-66.
    XU Yong, SHOU Linfei, YU Miao, XU Zhengning. UPLC-MS/MS method for determination of paclobutrazol, forchlorfenuron and prochloraz residues in fruits[J]. Chinese Journal of Pesticide Science, 2012, 14(1): 61-66.
    Citation: XU Yong, SHOU Linfei, YU Miao, XU Zhengning. UPLC-MS/MS method for determination of paclobutrazol, forchlorfenuron and prochloraz residues in fruits[J]. Chinese Journal of Pesticide Science, 2012, 14(1): 61-66.

    超高效液相色谱-串联四级杆质谱联用法测定水果中多效唑、氯吡脲和咪鲜胺的残留

    UPLC-MS/MS method for determination of paclobutrazol, forchlorfenuron and prochloraz residues in fruits

    • 摘要: 建立了超高效液相色谱-串联四级杆质谱(UPLC-MS/MS)法同时分析西瓜、杨梅中多效唑、氯吡脲和咪鲜胺3种农药残留的方法。样品经乙腈提取后用氨基固相萃取柱净化,反相液相色谱分离,采用三重四级杆串联质谱检测,用基质匹配标准品的外标法定量。结果表明:在添加水平为0.05~0.2 mg/kg范围时,西瓜中多效唑、氯吡脲和咪鲜胺的平均添加回收率分别为85.4%~99.4%、85.6%~98.7%和88.8%~100.3%,相对标准偏差(RSD)分别为2.7%~4.0%、2.5%~3.6%和2.3%~4.6%;杨梅中多效唑、氯吡脲、咪鲜胺的平均添加回收率分别为84.3%~99.3%、84.6%~98.2%和83.6%~99.2%, RSD 分别为2.4%~4.5%、2.9%~3.7%和2.2%~3.9%。该方法对两种水果中3种农药的检出限 (LOD)均为0.5 μg/kg,定量限(LOQ)均为1.7 μg/kg。方法灵敏度高、操作简便、定量准确、测定浓度范围宽,可用于多效唑、氯吡脲、咪鲜胺在西瓜、杨梅等水果中的残留分析。

       

      Abstract: A rapid method for determination of paclobutrazol,forchlorfenuron and prochloraz residues in watermelon and waxberry was established using ultra high-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS).The sample was extracted with acetonitrile and cleaned by solid phase extraction (SPE) cartridge.The mass spectrometer was operated with electrospray in the positive ion mode (ESI+).The target analytes were quantified by external standard method and matrix-matched standard solution used to compensate for matrix effect.Average recoveries of paclobutrazol,forchlorfenuron and prochloraz in watermelon samples were in the range of 85.4%-99.4%,85.6%-98.7% and 88.8%-100.3% at three spiking levels from 0.05-0.2 mg/kg with relative standard deviations of 2.7%-4.0%,2.5%-3.6% and 2.3%-4.6%.Average recoveries of paclobutrazol,forchlorfenuron and prochloraz in waxberry samples were found in the range of 84.3%-99.3%,84.6%-98.2% and 83.6%-99.2% at three spiking levels from 0.05-0.2 mg/kg with relative standard deviations of 2.4%-4.5%,2.9%-3.7% and 2.2%-3.9%.Limits of detections (LOD) of paclobutrazol,forchlorfenuron and prochloraz in fruits were 0.5,0.5 and 0.5 μg/kg,while limits of quantifications (LOQ) were 1.7,1.7 and 1.7 μg/kg.The method is simple and suitable for the routine and confirmation analysis on fruits.

       

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