| 第 50 卷第 3 期 |  | Vol. 50 No. 3 | | 2020 年 6 月 | Jun 2020 |
|
所属栏目：分析与测试
固相萃取／高效液相色谱-串联质谱法测定烟叶中春雷霉素残留量 |
| 张贵群1，2，3，郭素静4，梁贵平1，2，3，梁 骥1，2，3，刘义珂1，2，3，曾利红1，2，侯根连1，2，3
（1. 湖南化工研究院 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. 湖南加法检测有限公司，湖南 长沙 410014；4. 农业农村部农药检定所，北京 朝阳 100125） |
| 摘 要：建立了固相萃取／高效液相色谱-串联质谱（SPE／HPLC-MS／MS）测定烟叶中春雷霉素残留量的分析方法。样品经0.1%甲酸的甲醇水溶液（7∶3，v／v）超声提取后，采用混合型阳离子（PCX）小柱净化，以Kinetex PFP色谱柱分离，采用UPLC - MS／MS多反应监测（MRM）正离子模式测定，外标法定量。春雷霉素在烟叶中的最低检测浓度为0.05 mg·kg-1，在0.05、0.50、2.00 mg·kg-1 3个添加水平下，平均回收率为78%~87%，相对标准偏差为3%~8%。 |
| 关键词：高效液相色谱-串联质谱；春雷霉素；残留；烟叶 |
| 中图分类号：O657.7 文献标识码：A 文章编号：1009-9212（2020）03-0073-04 |
|
| 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 |
|
基金项目：国家药典委员会药品审评审批制度综合改革项目（ZG-2016-08）。
|
作者简介：张贵群（1984-），男，湖南郴州人，助理研究员，硕士，研究方向：农药残留分析及农残国家标准制定（E-mail：274702782@qq.com）。
|
收稿日期：2020-05-20
|
|