| 吴琴燕1, 5, 陈宏州1, 李冬冬2, 张文文3, 杨红福1, 庄义庆1, 4*.UPLC-MS/MS法检测麦穗中氟唑菌酰羟胺的残留和消解动态[J].植物保护,2021,47(2):164-168. |
| UPLC-MS/MS法检测麦穗中氟唑菌酰羟胺的残留和消解动态 |
| Degradation dynamics and residue analysis of pydiflumetofen in wheat by ultra-high performance liquid chromatography tandem mass spectrometry |
| 投稿时间：2019-12-25 修订日期：2020-03-15 |
| DOI：10.16688/j.zwbh.2019716 |
| 中文关键词: 氟唑菌酰羟胺 超高效液相色谱-串联质谱 麦穗 消解 |
| 英文关键词:pydiflumetofen UPLC-MS/MS wheat spikes degradation |
| 基金项目:句容市社会发展项目（SF2018589878） |
| 作者 | 单位 | E-mail | | 吴琴燕1, 5, 陈宏州1, 李冬冬2, 张文文3, 杨红福1, 庄义庆1, 4* | 1. 江苏丘陵地区镇江农业科学研究所中心实验室, 镇江212400
2. 江苏农林职业技术学院, 镇江212400
3. 江苏省镇江市农业农村局, 镇江212000
4. 江苏省农业科学院, 南京210014
5. 江苏省镇江市农业科学技术实业公司, 镇江212400 | 64816324@qq.com |
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| 中文摘要: |
| 建立了小麦扬花期和收获期麦穗中氟唑菌酰羟胺超高效液相色谱－串联质谱法(UPLC-MS/MS)检测方法, 明确了氟唑菌酰羟胺在小麦麦穗中的消解动态。试验结果表明, 在室温条件下, 当乙腈浓度为60%, 液固比为20 mL/g, 超声破碎时间为15 min, 扬花期和收获期样品中氟唑菌酰羟胺提取量均达到较高水平, 分别为3.34 μg/g和1.12 μg/g; 利用空白加标试验, 扬花期和收获期样品加标回收率为80.3%~115.8%, 方法的检出限为0.03 ng/mL, 定量限为0.15 ng/mL。氟唑菌酰羟胺在麦穗上的消解动态符合一级反应动力学方程, 半衰期为3.2~4.4 d。收获后麦粒中氟唑菌酰羟胺残留量为0.12 μg/g, 低于美国规定的农药残留限量标准（0.3 μg/g）。结果表明, 氟唑菌酰羟胺用于小麦病害防治是安全的。 |
| 英文摘要: |
| A ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed to determine the degradation dynamics of pydiflumetofen in wheat spikes at flowering and harvest stages, respectively. The results showed that, the extraction amount of pydiflumetofen from the samples at flowering and harvest stages all reached a higher level, when the concentration of acetonitrile was 60%, the liquid-solid ratio was 20 mL/g, and the ultrasonic breaking time was 15 minutes, which was 3.34 μg/g and 1.12 μg/g, respectively. The recovery rate of pydiflumetofen in fortified wheat spikes at flowering and harvest stages ranged from 80.3% to 115.8%; the detection limit (LOD) of the method was 0.03 ng/mL, and the quantitative limit (LQD) was 0.15 ng/mL. The digestion dynamics of pydiflumetofen residue with time accorded with first-order reaction kinetics equation. The half-life of pydiflumetofen in wheat spikes was 3.24.4 d. The residue of pydiflumetofen in wheat grains was 0.12 μg/g, which was lower than the maximum residue limit of the United States (0.3 μg/g). Therefore, pydiflumetofen is safe for wheat disease control. |
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