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      点此下载全文 HTML
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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杨庆喜 沈阳农业大学 植物保护学院, 沈阳 110866  
刘娜 沈阳农业大学 植物保护学院, 沈阳 110866  
张双 沈阳农业大学 植物保护学院, 沈阳 110866  
郝晏可 沈阳农业大学 植物保护学院, 沈阳 110866  
邹益泽 沈阳农业大学 植物保护学院, 沈阳 110866  
谷祖敏 沈阳农业大学 植物保护学院, 沈阳 110866 guzumin1212@163.com 
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
 
Determination of 4 pesticide residues in hazelnut by modified QuEChERS method using high performance liquid chromatography-tandem mass spectrometry
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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