2甲4氯异辛酯和氯氟吡氧乙酸异辛酯在冬小麦和土壤中的残留研究

doi:10.3969/j.issn.1004-616x.2021.05.011

癌变·畸变·突变 ›› 2021, Vol. 33 ›› Issue (5): 375-382.doi: 10.3969/j.issn.1004-616x.2021.05.011

2甲4氯异辛酯和氯氟吡氧乙酸异辛酯在冬小麦和土壤中的残留研究

杜月梅^1,2, 邵华², 高丽萍¹

1. 北京联合大学生物化学工程学院生物活性物质与功能食品北京市重点实验室, 北京 100191;
2. 中国农业科学院农业质量标准与检测技术研究所, 北京 100081

收稿日期:2020-11-08 修回日期:2020-12-30 出版日期:2021-09-30 发布日期:2021-10-09
通讯作者: 邵华,E-mail:nkshaohua@163.com;高丽萍,E-mail:gaolip62@163.com E-mail:nkshaohua@163.com;gaolip62@163.com
作者简介:杜月梅,E-mail:1046655264@qq.com。
基金资助:
国家重点研发计划项目（2019YFC1605601）；中央级公益性科研院所基本科研业务费专项资助（1610072020004）

Determination of MCPA-isooctyl and fluroxypyr-methyl residues in winter wheat and soil

DU Yuemei^1,2, SHAO Hua², GAO Liping¹

1. Beijing Key Laboratory of Bioactive Substances and Functional Foods, School of Biochemical Engineering, Beijing Union University, Beijing 100191;
2. Institute of Quality Standard and Testing Technology for Groproducts, Chinese Academy of Agricultural Sciences, Beijing 100081, China

Received:2020-11-08 Revised:2020-12-30 Online:2021-09-30 Published:2021-10-09

摘要/Abstract

摘要： 目的：为确保2甲4氯异辛酯、氯氟吡氧乙酸异辛酯的安全使用，探讨其在小麦上的消解趋势以及残留水平。方法：试验分麦粒、植株和土壤3组，进行评价48% 2甲4氯异辛酯·氯氟吡氧乙酸异辛酯·双氟磺草胺悬浮剂在小麦上的残留动态及最终残留水平的两年三地残留试验。分别采用高效液相色谱-质谱法和气相色谱-质谱法检测3组样品中的2甲4氯异辛酯和氯氟吡氧乙酸异辛酯的消解动态及最终残留。3组样品经乙腈提取，上清液经分散固相萃取净化后，过膜，气相色谱-质谱法和高效液相色谱－串联质谱法进行检测，外标法定量。结果：小麦、植株和土壤基质中，2甲4氯异辛酯在0.005~0.2 mg/kg，氯氟吡氧乙酸异辛酯在0.02~0.2 mg/kg范围内其检出浓度和添加水平呈线性关系，在0.05、0.1、0.2 mg/kg 3个添加水平下，其回收率为77.0%~112.0%，相对标准偏差为1.1%~9.9%，定量检出限（LOQ）为0.05 mg/kg。在两年（2016—2017年）三地（北京、河南、宁夏）的消解动态实验中，氯氟吡氧乙酸异辛酯在2016年北京小麦植株上的消解半衰期t_1/2为5.92 d，在2016年北京、2017年宁夏的土壤实验中t_1/2分别为1.56、9.63 d，其他时间和地点在小麦植株和土壤的实验均无法得出消解动态的动力学曲线方程。收获小麦中2甲4氯异辛酯和氯氟吡氧乙酸异辛酯的最终残留量均<0.05 mg/kg，低于国家规定的小麦中这两种农药的最大残留限量值。结论：2甲4氯异辛酯和氯氟吡氧乙酸异辛酯在冬小麦和土壤中的消解速度较快，因此，48% 2甲4氯异辛酯·氯氟吡氧乙酸异辛酯·双氟磺草胺悬浮剂在推荐剂量（432 ga.i./hm²）下施用不会造成小麦、土壤的残留污染。

关键词: 2甲4氯异辛酯, 氯氟吡氧乙酸异辛酯, 气相色谱-质谱法, 高效液相色谱-串联质谱法, 小麦

Abstract: OBJECTIVE: To evaluate safety of MCPA-isooctyl and fluroxypyr-meptyl based on their digestion trends and residual levels on wheat. METHODS: The residue dynamics and final residue levels of 48% MCPA-isooctyl · fluroxypyr-meptyl · sulfentrazone suspension concentrates on wheat were carried out in three places for two years. The investigation involving three groups:wheat grain, plant and soil, and the digestion dynamics of MCPA-isooctyl and fluroxypyr-meptyl, were detected using high performance liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry. The three sets of samples were extracted with acetonitrile, the supernatant was purified by dispersive solid phase extraction, passed through the membrane,detected by gas chromatography-mass spectrometry and high-performance liquid chromatographytandem mass spectrometry,and also quantified by external standard method. RESULTS: The MCPA-isooctyl in wheat,plants and soil microorganisms was in the range of 0.005-0.2 mg/kg,and the fluroxypyr-meptyl in the range of 0.02-0.2 mg/kg. They showed a linear relationship with 0.05,0.1,0.2 mg/kg at 3 addition levels. The recovery rates were 77.0%-112.0%,the relative standard deviations were 1.1%-9.9%,and the limit of quantitative detection (LOQ) was 0.05 mg/kg. In 2 years (2016-2017) and in 3 places (Beijing, Henan, Ningxia), the digestion dynamic investigations show that the digestion half-life t_1/2 of fluroxypyr-meptyl on wheat plants in Beijing in 2016 was 5.92 d. In the soil samples in Beijing (2016) and Ningxia (2017),t_1/2 were 1.56 and 9.63 d,respectively. For comparison,the final residues of MCPA-isooctyl in wheat which were harvested at other times and other locations were <0.05 mg/kg. The final residues of fluroxypyr-meptyl were < 0.05 mg/kg which were lower than the national maximum residue limits for these two pesticides in wheat. CONCLUSION: MCPA-isooctyl and fluroxypyr-meptyl in winter wheat and soil had faster digestion rates. Therefore, 48% MCPA-isooctyl · fluroxypyr-meptyl · difluoro sulfentrazone suspension at the recommended dosage of 432 ga.i./hm² would probably not cause residual contamination of wheat and soil.

Key words: MCPA-isooctyl, fluroxypyr-meptyl, gas chromatography-mass spectrometry, high performance liquid chromatography-tandem mass spectrometry, wheat

中图分类号:

杜月梅, 邵华, 高丽萍. 2甲4氯异辛酯和氯氟吡氧乙酸异辛酯在冬小麦和土壤中的残留研究[J]. 癌变·畸变·突变, 2021, 33(5): 375-382.

DU Yuemei, SHAO Hua, GAO Liping. Determination of MCPA-isooctyl and fluroxypyr-methyl residues in winter wheat and soil[J]. Carcinogenesis, Teratogenesis & Mutagenesis, 2021, 33(5): 375-382.

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2甲4氯异辛酯和氯氟吡氧乙酸异辛酯在冬小麦和土壤中的残留研究

Determination of MCPA-isooctyl and fluroxypyr-methyl residues in winter wheat and soil

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