| 第 50 卷第 3 期 |  | Vol. 50 No. 3 | | 2020 年 6 月 | Jun 2020 |
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所屬欄目：分析與測試
固相萃�。咝б合嗌V-串聯(lián)質(zhì)譜法測定煙葉中春雷霉素殘留量 |
| 張貴群1，2，3，郭素靜4，梁貴平1，2，3，梁 驥1，2，3，劉義珂1，2，3，曾利紅1，2，侯根連1，2，3
（1. 湖南化工研究院 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. 農業(yè)農村部農藥檢定所，北京 朝陽(yáng) 100125） |
| 摘 要：建立了固相萃�。咝б合嗌V-串聯(lián)質(zhì)譜（SPE／HPLC-MS／MS）測定煙葉中春雷霉素殘留量的分析方法。樣品經(jīng)0.1%甲酸的甲醇水溶液（7∶3，v／v）超聲提取后，采用混合型陽(yáng)離子（PCX）小柱凈化，以Kinetex PFP色譜柱分離，采用UPLC - MS／MS多反應監測（MRM）正離子模式測定，外標法定量。春雷霉素在煙葉中的最低檢測濃度為0.05 mg·kg-1，在0.05、0.50、2.00 mg·kg-1 3個(gè)添加水平下，平均回收率為78%~87%，相對標準偏差為3%~8%。 |
| 關(guān)鍵詞：高效液相色譜-串聯(lián)質(zhì)譜；春雷霉素；殘留；煙葉 |
| 中圖分類(lèi)號：O657.7 文獻標識碼：A 文章編號：1009-9212（2020）03-0073-04 |
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| Determination of Kasugamycin Residues in Fresh and Cured Tobacco Leaves by Solid Phase Extraction/High Performance Liquid Chromatography Tandem Mass Spectrometry |
| High Performance Liquid Chromatography Tandem Mass Spectrometry
ZHANG Gui-qun1,2,3, GUO Su-jing4, LIANG Gui-ping1,2,3, LIANG Ji1,2,3, LIU Yi-ke1,2,3, ZENG Li-hong1,2, HOU Gen-lian1,2,3
(1. National Engineering Research Center for Agrochemicals, Hunan Research Institute of Chemical Industry Changsha 410014, China; 2. Hunan Province Key Laboratory for Agrochemicals, Changsha 410014, China; 3. Hunan J&F Test Co.,Ltd., Changsha, 410014, China; 4. Institute for the Control of Agrochemicals, Ministry of Agriculture and Rural Affairs, Beijing 100125, China) |
| Abstract：A method of determination for kasugamycin in tobacco leaves by HPLC-MS/MS was established. The analytes were extracted from samples using 0.1% formic acid methanol and water solution（7+3, v/v）, and purified with PCX solid phase extraction columns, then analyzed using UPLC-MS/MS multiple reaction monitoring (MRM) mode via positive electrospray ionization with a Waters Kinetex PFP column as the analytical column. All the analytes were quantified by the external standard method. The limit of quantification was 0.05 mg·kg-1. The results showed that the average recoveries at the fortified levels of 0.05, 0.50, 2.00 mg·kg-1 ranged from 78% to 87%, and the RSD were 3%~8%. |
| Key words：HPLC-MS/MS; kasugamycin; residue; tobacco leaves |
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基金項目：國家藥典委員會(huì )藥品審評審批制度綜合改革項目（ZG-2016-08）。
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作者簡(jiǎn)介：張貴群（1984-），男，湖南郴州人，助理研究員，碩士，研究方向：農藥殘留分析及農殘國家標準制定（E-mail：274702782@qq.com）。
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收稿日期：2020-05-20
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