杨庆喜, 刘娜, 张双, 郝晏可, 邹益泽, 谷祖敏. QuEChERS-高效液相色谱-串联质谱法测定榛子中4种农药的残留[J]. 农药学学报, 2018, 20(6): 776-782. DOI: 10.16801/j.issn.1008-7303.2018.0098
    引用本文: 杨庆喜, 刘娜, 张双, 郝晏可, 邹益泽, 谷祖敏. QuEChERS-高效液相色谱-串联质谱法测定榛子中4种农药的残留[J]. 农药学学报, 2018, 20(6): 776-782. DOI: 10.16801/j.issn.1008-7303.2018.0098
    YANG Qingxi, LIU Na, ZHANG Shuang, HAO Yanke, ZOU Yize, GU Zumin. Determinationof4pesticideresiduesinhazelnutbymodifiedQuEChERSmethodusinghighperformanceliquidchromatography-tandemmassspectrometry[J]. Chinese Journal of Pesticide Science, 2018, 20(6): 776-782. DOI: 10.16801/j.issn.1008-7303.2018.0098
    Citation: YANG Qingxi, LIU Na, ZHANG Shuang, HAO Yanke, ZOU Yize, GU Zumin. Determinationof4pesticideresiduesinhazelnutbymodifiedQuEChERSmethodusinghighperformanceliquidchromatography-tandemmassspectrometry[J]. Chinese Journal of Pesticide Science, 2018, 20(6): 776-782. DOI: 10.16801/j.issn.1008-7303.2018.0098

    QuEChERS-高效液相色谱-串联质谱法测定榛子中4种农药的残留

    Determinationof4pesticideresiduesinhazelnutbymodifiedQuEChERSmethodusinghighperformanceliquidchromatography-tandemmassspectrometry

    • 摘要: 建立了同时检测榛子中苯醚甲环唑、丙环唑、噻虫嗪和啶虫脒4种农药残留量的QuEChERS-高效液相色谱-串联质谱 (HPLC-MS/MS) 检测方法。榛仁和榛壳分别经正己烷饱和的乙腈和乙腈提取,用弗罗里硅土、石墨化碳黑 (GCB) 和N-丙基乙二胺 (PSA) 净化。C18色谱柱分离,采用电喷雾正离子 (ESI+) 扫描,在多重反应监测 (MRM) 模式下进行质谱分析,外标法定量。结果表明:在0.01~2 mg/kg范围内,苯醚甲环唑、丙环唑、噻虫嗪和啶虫脒4种供试农药的质量浓度与对应的峰面积间呈良好线性关系 (R2 > 0.990 2)。在0.01、0.1和1 mg/kg 3个添加水平下,4 种农药在榛子中的日内平均回收率为79%~111%,相对标准偏差 (RSDs) (n = 5) 为0.6%~6.9%,日间平均回收率为81%~110%,RSDs (n = 15) 为1.1%~8.5%。4种农药的定量限均为0.01 mg/kg。此方法简单、高效,可为榛子等坚果类食品中多种农药残留的同时测定提供参考。

       

      Abstract: A multi-residue analysis method was developed for the determination of 4 pesticide (difenoconazole, propiconazole, thiamethoxam and acetamiprid) residues in hazelnut (including the nut and shell) based on a QuEChERS procedure using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The samples (hazelnut, and the hazelnut shell) were extracted with hexane-saturated acetonitrile and acetonitrile, and cleaned-up by florisil, GCB and PSA. The samples were separated by using an eclipse plus C18 column connected to an electrospray ionization source in positive mode (ESI+), and analyzed by multiple reaction monitoring (MRM) mode. The external standard method was employed for the quantification. The results indicated that in the linear ranged from 0.01 to 2 mg/kg, all pesticides have a good linear relationship. At three spiked levels (0.01, 0.1 and 1 mg/kg), the intra-day average recoveries of 4 pesticides ranged from 79% to 111%, and the relative standard deviation (RSDs) ranged from 0.6% to 6.9% (n = 5), while the inter-day average recoveries ranged from 81% to 110%, and the RSDs ranged from 1.1% to 8.5% (n = 15). The limits of quantitation (LOQ) of 4 pesticides were all 0.01 mg/kg .This method is simple and highly efficient, which could be used for the routine analysis of the four pesticide residues in hazelnut.

       

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