精细化工中间体2024,Vol.54Issue(1) :79-84.DOI:10.19342/j.cnki.issn.1009-9212.2024.01.017

液相色谱-串联质谱法同时测定水稻中乙氧磺隆和双环磺草酮的残留量

Determination of Ethoxysulfuron and Benzobicyclon in Rice by LC-MS/MS

张港 胡军和 曾利红 侯根连 欧晓明 金晨钟
精细化工中间体2024,Vol.54Issue(1) :79-84.DOI:10.19342/j.cnki.issn.1009-9212.2024.01.017

液相色谱-串联质谱法同时测定水稻中乙氧磺隆和双环磺草酮的残留量

Determination of Ethoxysulfuron and Benzobicyclon in Rice by LC-MS/MS

张港 1胡军和 1曾利红 2侯根连 2欧晓明 2金晨钟1
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作者信息

  • 1. 湖南人文科技学院农药无害化应用重点实验室,湖南省农田杂草防控技术与应用协同创新中心,湖南娄底417000
  • 2. 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;农用化学品湖南省重点实验室,湖南长沙410014;湖南安全生产科学研究有限公司,湖南长沙410014
  • 折叠

摘要

建立液相色谱—串联质谱法(LC-MS/MS)检测乙氧磺隆和双环磺草酮在水稻中残留分析方法.样品经乙腈溶液涡旋提取,NaCl盐析,0.25gMgSO4、0.05 gPSA和0.05gC18净化后,采用电喷雾离子源正离子扫描,多反应监测(MRM)模式下,外标法定量.结果表明:在0.001~0.5 μg/mL范围内线性关系良好,相关系数(R2)>0.99.当添加浓度为0.01~1.0 mg/kg时,在糙米中的平均回收率为84%~107%,相对标准偏差为1%~8%.当添加浓度为0.05~2.5 mg/kg时,在0.001~0.5 μg/mL范围内线性关系良好,相关系数(R2)>0.99.在稻壳中的平均回收率为86%~101%,相对标准偏差为2%~8%;在秸秆中的平均回收率为87%~99%,相对标准偏差为6%~11%.乙氧磺隆和双环磺草酮在糙米中的定量限为0.01 mg/kg,在稻壳和秸秆中的定量限为0.05 mg/kg.

Abstract

To establish a method for simultaneous ethoxysulfuron and benzobicyclon residues in rice by LC-MS/MS.The samples were vortexed with acetonitrile solution,NaCl salted out,purified with 0.25 g MgSO4,0.05 g PSA and 0.05 g C18,electrelectrospray ionization(ESI+)positive ion scanning,multiple reaction monitoring(MRM)mode,and external standard method.The results showed that the correlation coefficient of 2 pesticides were higher than 0.99 in the concentration ranged from 0.001 to 0.5 µg/L.When the spiked level ranged from 0.01 to 1.0 mg/kg,the average recovery rates of 2 pesticides in rice ranged from 84%to 107%,and the RSD ranged from 1%to 8%.When the spiked level ranged from 0.05 to 2.5 mg/kg,the average recovery rates of 2 pesticides in rice hull ranged from 86%to 101%,and the RSD ranged from 2%to 8%;in rice plant ranged from 87%to 99%,and the RSD ranged from 6%to 11%.The limits of quantitation of ethoxysulfuron and benzobicyclon in rice samples were 0.01 mg/kg and in rice hull and rice plant samples were 0.05 mg/kg.

关键词

LC-MS/MS/乙氧磺隆/双环磺草酮/水稻/残留检测

Key words

LC-MS/MS/ethoxysulfuron/benzobicyclon/rice/residue determination

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出版年

2024
精细化工中间体
湖南化工研究院

精细化工中间体

CSTPCD
影响因子:0.236
ISSN:1009-9212
参考文献量17
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