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第 50 卷第 5 期Vol. 50 No. 5
2020 年 10 月Oct 2020

所屬欄目:分析與測試

UPLC-MS/MS測定西瓜中噁霉靈和吡唑醚菌酯的殘留量
侯根連1,2,3,曾利紅1,2,3,俞 泉4 (1.湖南化工研究院有限公司 國家農藥創(chuàng )制工程技術(shù)研究中心,湖南 長(cháng)沙410014;2.農用化學(xué)品湖南省重點(diǎn)實(shí)驗室,湖南 長(cháng)沙 410014;3.湖南加法檢測有限公司,湖南 長(cháng)沙410014;4.湖南人文科技學(xué)院,湖南 婁底 417000)
摘 要:建立了超高效液相色譜-串聯(lián)質(zhì)譜(UPLC-MS/MS)快速測定西瓜中噁霉靈、吡唑醚菌酯殘留量的方法。樣品用乙腈提取,過(guò)0.22 μm有機系濾膜,以0.1%甲酸水溶液-乙腈為流動(dòng)相梯度洗脫,多反應監測(MRM)模式下,正離子掃描,外標法定量。結果表明:方法在0.001~0.1 μg·mL-1范圍內線(xiàn)性良好,相關(guān)系數(R2)>0.99;在0.02、0.5、2.0 mg·kg-1 3個(gè)添加水平下,噁霉靈和吡唑醚菌酯的平均回收率分別為96%~109%和90%~99%,相對標準偏差分別為1%~3%和1%~4%,定量限為0.005 mg·kg-1。
關(guān)鍵詞:UPLC-MS/MS;噁霉靈;吡唑醚菌酯;西瓜;殘留檢測
中圖分類(lèi)號:O657.7  文獻標識碼:A  文章編號:1009-9212(2020)05-0073-04
Determination of Hymexazol and Pyraclostrobin in Watermelon by UPLC-MS/MS
HOU Gen-lian1,2,3, ZENG Li-hong1,2,3, YU Quan4 (1. National Engineering Research Center for Agrochemicals, Hunan Research Institute of Chemical Industry Co.,Ltd., Changsha 410014, China; 2. Hunan Province Key Laboratory for Agrochemicals, Changsha 410014, China; 3. Hunan J&F Test Co., Ltd., Changsha 410014, China; 4. Hunan University of Humanities, Science and Technology, Loudi 417000, China)
Abstract:A method for rapid determination of Hymexazol and Pyraclostrobin in watermelon by ultra high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was established. Samples were prepared through extraction using acetonitrile followed by filtration using 0.22 μm organic filtration membrane. 0.1% formic acid water/acetonitrile was used as mobile phase and the multi-reaction monitoring (MRM) mode was used to measure the samples. The results showed that the linear range of the method was 0.001~0.1 mg·kg-1, and the determination coefficient (R2) was more than 0.99. At the three levels including 0.02, 0.5 and 2.0 mg·kg-1, the average recovery of the Hymexazol and Pyraclostrobin was 96%~109% and 90%~99% , the RSD were 1%~3% and 1%~4%. The limit of quantification was 0.005 mg·kg-1.
Key words:UPLC-MS/MS; Hymexazol; Pyraclostrobin; watermelon; detecting residues
基金項目:國家自然科學(xué)基金項目(21572050)。
作者簡(jiǎn)介:侯根連(1979—),女,山西平遙人,主要從事農藥殘留分析(E-mail:76251033@qq.com)。
收稿日期: 2020-08-1
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