【摘要】：目的建立超高效液相色譜-高分辨質(zhì)譜同時(shí)快速測(cè)定蜂蜜中14種農(nóng)藥殘留的方法。方法樣品采用1%甲酸乙腈提取,以N-丙基乙二胺(PSA)和C18作為吸附劑的分散固相萃取法(d-SPE)進(jìn)行凈化,以Accucore a Q C18色譜柱(2.6μm,2.1 mm×150 mm)進(jìn)行色譜分離,通過高分辨質(zhì)譜的全掃描/實(shí)時(shí)二級(jí)質(zhì)譜掃描模式進(jìn)行定性篩查和定量檢測(cè)。結(jié)果 14種農(nóng)藥殘留在一定濃度范圍內(nèi)呈良好的線性關(guān)系,相關(guān)系數(shù)(r)均大于0.998,定量限(LOQ)為0.6~6μg/kg。空白蜂蜜樣品在LOQ、15和30μg/kg三個(gè)加標(biāo)水平的平均回收率為80.3%~112.7%,相對(duì)標(biāo)準(zhǔn)偏差為0.4%~7.1%。結(jié)論該方法適合蜂蜜中農(nóng)藥多殘留的快速篩查和定量。
[Abstract]:Objective to establish a rapid method for the simultaneous determination of 14 pesticide residues in honey by high performance liquid chromatography-high resolution mass spectrometry. Methods the samples were extracted with 1% acetonitrile formate and purified by dispersive solid-phase extraction (d-SPE) with N-propylethylenediamine (PSA) and C18 as adsorbents, and separated by Accucore a Q C _ (18) column (2.6 渭 m ~ (2.1) mm 脳 150 mm). Qualitative screening and quantitative detection were carried out by high resolution mass spectrometry (HRMS) full scan / real-time second-stage mass spectrometry scanning mode. Results there was a good linear relationship between the 14 pesticide residues in a certain concentration range, the correlation coefficient (r) was greater than 0.998, and the quantitative limit (LOQ) was 0.6 渭 g / kg. The average recoveries of blank honey samples at LOQ,15 and 30 渭 g/kg levels were 80.3 and 112.7, and the relative standard deviation was 0.4 and 7.1. Conclusion this method is suitable for rapid screening and quantification of pesticide residues in honey.
【作者單位】： 國家食品安全風(fēng)險(xiǎn)評(píng)估中心
【基金】：國家國際科技合作專項(xiàng)(No.2011DFA31770)
【分類號(hào)】：R155.5

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本文編號(hào)：2400428