第 52 卷第 3 期Vol. 52 No. 3
2022 年 6 月Jun 2022
所属栏目：分析与测试

高效液相色谱-串联质谱法测定水稻中稻瘟灵和噁霉灵残留量
宋强勇1，2，3，晏 姣1，2，3*，曾利红1，2，3，袁桂平4，侯根连1，2，3，梁贵平1，2，3，聂春林1，2，3 （1.湖南化工研究院有限公司 国家农药创制工程技术研究中心，湖南 长沙 410014；2.农用化学品湖南省重点实验室，湖南 长沙 410014；3.湖南化研院检测技术有限公司，湖南 长沙 410014；4.常德市西湖管理区农业农村局，湖南 常德 415921）
摘　要：建立了高效液相色谱-串联质谱（HPLC-MS/MS）测定水稻中稻瘟灵和噁霉灵残留量的分析方法。样品中稻瘟灵和噁霉灵用乙腈水溶液（V∶V=1∶1）提取，经HC-C18净化，以Agilent Proshell 120 EC-C8色谱柱分离，采用HPLC-MS/MS多反应监测（MRM）正离子模式测定，外标法定量。结果表明：在1~100 ng/mL的质量浓度范围内，稻瘟灵和噁霉灵的峰面积与质量浓度之间呈现出良好的线性关系；稻瘟灵和噁霉灵在水稻稻壳和水稻秸秆中的最低检测浓度均为0.05 mg/kg，在水稻糙米中的最低检测浓度为0.02 mg/kg。在添加浓度为0.05~2.0 mg/kg时，稻瘟灵和噁霉灵在水稻稻壳中的平均加标回收率为86%~103%，相对标准偏差为3%~10%；在水稻秸秆中的平均加标回收率为84%~107%，相对标准偏差为2%~7%。在添加浓度为0.02~2.0 mg/kg时，稻瘟灵和噁霉灵在水稻糙米中的平均加标回收率为91%~108%，相对标准偏差为1%~15%。该方法快速简便、准确可靠，可用于水稻中稻瘟灵和噁霉灵的残留量检测。
关键词：稻瘟灵；噁霉灵；高效液相色谱-串联质谱；水稻；残留
中图分类号：TQ455　　文献标识码：A　　文章编号：1009-9212（2022）03-0077-05
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
作者简介：宋强勇（1974—），女，湖南湘潭人，研究方向：农药残留化学研究（E-mail：1483040867@qq.com）。
联 系 人：晏 姣，工程师，研究方向：农药残留化学研究（E-mail：1120969160@qq.com）。
收稿日期：2022-03-09