QuEChERS-高效液相色谱-串联质谱法测定榛子中4种农药的残留 |
投稿时间:2018-07-20
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引用本文:杨庆喜,刘娜,张双,等.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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中文摘要: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。 |
中文关键词: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 |
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Determination of 4 pesticide residues in hazelnut by modified QuEChERS method using high performance liquid chromatography-tandem mass spectrometry |
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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. |
Key words:QuEChERS high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) hazelnut difenoconazole propiconazole thiamethoxam acetamiprid residue |
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