首页|超高效液相色谱-串联质谱测定谷子、植株和土壤中的单嘧磺隆残留

超高效液相色谱-串联质谱测定谷子、植株和土壤中的单嘧磺隆残留

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[目的]单嘧磺隆是我国创制的谷子田内吸型磺酰脲类除草剂,在谷子田应用前景广阔.采用超高效液相色谱串联质谱法(UPLC-MS/MS)建立了谷子、植株和土壤中单嘧磺隆的残留检测方法,并测定了收获期的残留量,为单嘧磺隆的安全使用提供技术支撑.[方法]谷子、植株和土壤中的单嘧磺隆残留采用纯乙腈振荡提取,C18和GCB净化,UPLC-MS/MS检测,外标法定量.[结果]在0.0025~0.1 mg/L质量浓度范围内,单嘧磺隆质量浓度与其峰面积之间呈现出良好线性关系,R2≥0.9984.在0.005、0.01、0.1 mg/kg添加水平,单嘧磺隆在谷子、植株和土壤中的回收率在69%~96%范围内,相对标准偏差低于12.1%,符合农药残留分析的要求.田间条件下,按照推荐剂量施用10%单嘧磺隆可湿性粉剂,收获期谷子、植株和土壤中单嘧磺隆残留均低于方法的定量限(LOQ,0.005 mg/kg).[结论]10%单嘧磺隆可湿性粉剂按照推荐剂量施用收获期安全.本试验可以为单嘧磺隆的安全使用和最大残留限量(MRL)的制定提供基础数据.
Determination of monosulfuron residue in millet,straw and soil by ultra-high performance liquid chromatography-tandem mass spectrometry
[Aims]Monosulfuron is a new systemic sulfonylurea herbicide for millet field registered in China.It has broad application prospects in millet fields.A method for detecting monosulfuron residue in millet,straw and soil was established using ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS),and the residue during the harvest period was determined,which will provide guidance for the safe use of monosulfuron.[Methods]Monosulfuron residue in millet,straw and soil were extracted with acetonitrile,purified with C18 and GCB,detected by UPLC-MS/MS,and quantified by the external standard method.[Results]In the concentration range of 0.0025-0.1 mg/L,monosulfuron showed good linear relationship with R2≥0.9984.At the spiked levels of 0.005,0.01 and 0.1 mg/kg,the recoveries of monosulfuron in millet,straw and soil were ranged from 69%to 96%,with RSD less than 12.1%,meeting the requirements for residue analysis.Under field conditions,when monosulfuron 10%wettable powder was applied according to the recommended dose,the monosulfuron residue in millet,straw and soil during the harvest period were lower than the LOQ(0.005 mg/kg).[Conclusions]Monosulfuron 10%wettable powder is safe during the harvest period when applied at the recommended dose.This study can provide basic data for the safe use and the constitution of maximum residue limits(MRL)of monosulfuron.

monosulfuronmilletresidueultra-high performance liquid chromatography-tandem mass spectrometry

王彬、郭亚彬、秦曙、李晋栋、齐艳丽、任鹏程、曹俊丽

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山西农业大学山西功能农产品检验检测中心,太原 030031

山西大学生命科学学院,太原 030006

单嘧磺隆 谷子 残留 超高效液相色谱-串联质谱

山西省高等学校科技创新项目山西省基础研究计划青年项目山西农业大学博士科研启动项目

2022L0792021030212231492021BQ127

2024

农药
沈阳化工研究院有限公司

农药

CSTPCD北大核心
影响因子:0.665
ISSN:1006-0413
年,卷(期):2024.63(1)
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