| 第 52 卷第 3 期 |  | Vol. 52 No. 3 | | 2022 年 6 月 | Jun 2022 |
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所屬欄目：分析與測試
高效液相色譜-串聯(lián)質(zhì)譜法測定水稻中稻瘟靈和噁霉靈殘留量 |
| 宋強勇1，2，3，晏 姣1，2，3*，曾利紅1，2，3，袁桂平4，侯根連1，2，3，梁貴平1，2，3，聶春林1，2，3
（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.湖南化研院檢測技術(shù)有限公司，湖南 長(cháng)沙 410014；4.常德市西湖管理區農業(yè)農村局，湖南 常德 415921） |
| 摘 要：建立了高效液相色譜-串聯(lián)質(zhì)譜（HPLC-MS/MS）測定水稻中稻瘟靈和噁霉靈殘留量的分析方法。樣品中稻瘟靈和噁霉靈用乙腈水溶液（V∶V=1∶1）提取，經(jīng)HC-C18凈化，以Agilent Proshell 120 EC-C8色譜柱分離，采用HPLC-MS/MS多反應監測（MRM）正離子模式測定，外標法定量。結果表明：在1~100 ng/mL的質(zhì)量濃度范圍內，稻瘟靈和噁霉靈的峰面積與質(zhì)量濃度之間呈現出良好的線(xiàn)性關(guān)系；稻瘟靈和噁霉靈在水稻稻殼和水稻秸稈中的最低檢測濃度均為0.05 mg/kg，在水稻糙米中的最低檢測濃度為0.02 mg/kg。在添加濃度為0.05~2.0 mg/kg時(shí)，稻瘟靈和噁霉靈在水稻稻殼中的平均加標回收率為86%~103%，相對標準偏差為3%~10%；在水稻秸稈中的平均加標回收率為84%~107%，相對標準偏差為2%~7%。在添加濃度為0.02~2.0 mg/kg時(shí)，稻瘟靈和噁霉靈在水稻糙米中的平均加標回收率為91%~108%，相對標準偏差為1%~15%。該方法快速簡(jiǎn)便、準確可靠，可用于水稻中稻瘟靈和噁霉靈的殘留量檢測。 |
| 關(guān)鍵詞：稻瘟靈；噁霉靈；高效液相色譜-串聯(lián)質(zhì)譜；水稻；殘留 |
| 中圖分類(lèi)號：TQ455 文獻標識碼：A 文章編號：1009-9212（2022）03-0077-05 |
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| etermination of Isoprothiolane and Hymexazol Residues in Rice Using High Performance Liquid Chromatography Tandem Mass Spectrometry |
| SONG Qiang-yong1,2,3,YAN Jiao1,2,3*, ZENG Li-hong1,2,3, YUAN Gui-ping4, HOU Gen-lian1,2,3, LIANG Gui-ping1,2,3, NIE Chun-lin1,2,3
(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 Research Institute of Chemical Industry Testing Technology Co., Ltd., Changsha 410014, China; 4. Agriculture and Rural Affairs Bureau of West Lake Management District, Changde 415921, China) |
| Abstract：A method for the determination of isoprothiolane and hymexazol in rice by HPLC-MS/MS was established. The isoprothiolane and hymexazol residues in rice samples were extracted with a solution of acetonitrile and water (V∶V=1∶1), and purified by HC-C18, then analyzed using HPLC-MS/MS multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI+) with a Agilent Proshell 120 EC-C8 column as the analytical column. All the analytes were quantified by the external standard method. The results showed that there were in good linearity between the concentrations of isoprothiolane and hymexazol and their corresponding response values within a concentration range of 1~100 ng/mL, and the LOQ of isoprothiolane and hymexazol in rice hull and rice plant samples were 0.05 mg/kg and in rice samples were 0.02 mg/kg. When the spiked level ranged from 0.05 to 2.0 mg/kg, the average recovery rates of isoprothiolane and hymexazol in rice hull ranged from 86% to 103%, and the RSD ranged from 3% to 10%; the average recovery rates of isoprothiolane and hymexazol in rice plant ranged from 84% to 107%, and the RSD ranged from 2% to 7%. When the spiked level ranged from 0.02 to 2.0 mg/kg, the average recovery rates of isoprothiolane and hymexazol in rice ranged from 91% to 108%, and the RSD ranged from 1% to 15%. This method is rapid, simple and accurate, and can be used for the determination of isoprothiolane and hymexazol residues in rice samples. |
| Key words：isoprothiolane; hymexazol; HPLC-MS/MS; rice; residue |
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作者簡(jiǎn)介：宋強勇（1974—），女，湖南湘潭人，研究方向：農藥殘留化學(xué)研究（E-mail：1483040867@qq.com）。
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聯(lián) 系 人：晏 姣，工程師，研究方向：農藥殘留化學(xué)研究（E-mail：1120969160@qq.com）。
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收稿日期：2022-03-09
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