| QuEChERS-高效液相色谱-串联质谱法测定榛子中4种农药的残留 |
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| 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. |
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| 作者姓名： | 杨庆喜 刘娜 张双 郝晏可 邹益泽 谷祖敏 |
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| 作者单位： | 沈阳农业大学 植物保护学院，沈阳 110866 |
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| 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。
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| 关 键 词： | QuEChERS 高效液相色谱-串联质谱 榛子 苯醚甲环唑 丙环唑 噻虫嗪 啶虫脒 残留 |
| 收稿时间： | 2018/7/20 0:00:00 |
Determination of 4 pesticide residues in hazelnut by modified QuEChERS method using high performance liquid chromatography-tandem mass spectrometry |
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| YANG Qingxi,LIU N,ZHANG Shuang,HAO Yanke,ZOU Yize and GU Zumin.Determination of 4 pesticide residues in hazelnut by modified QuEChERS method using high performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Pesticide Science,2018,20(6):776-782. |
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| Authors: | YANG Qingxi LIU N ZHANG Shuang HAO Yanke ZOU Yize and GU Zumin |
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| Institution: | College of Plant Protection, Shenyang Agricultural University, Shenyang 110866, China |
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| 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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| Keywords: | QuEChERS high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) hazelnut difenoconazole propiconazole thiamethoxam acetamiprid residue |
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