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中国精品科技期刊2020
郭爱静, 花中霞, 辛佳, 张弘, 张世勇, 曹丽玲, 王可. 超高效液相色谱-串联质谱法测定油料作物中8种苯胺类除草剂[J]. 食品工业科技, 2021, 42(2): 204-209. DOI: 10.13386/j.issn1002-0306.2020040145
引用本文: 郭爱静, 花中霞, 辛佳, 张弘, 张世勇, 曹丽玲, 王可. 超高效液相色谱-串联质谱法测定油料作物中8种苯胺类除草剂[J]. 食品工业科技, 2021, 42(2): 204-209. DOI: 10.13386/j.issn1002-0306.2020040145
GUO Aijing, HUA Zhongxia, XIN Jia, ZHANG Hong, ZHANG Shiyong, CAO Liling, WANG Ke. Determination of 8 Aniline Herbicides in Oil Crops by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(2): 204-209. DOI: 10.13386/j.issn1002-0306.2020040145
Citation: GUO Aijing, HUA Zhongxia, XIN Jia, ZHANG Hong, ZHANG Shiyong, CAO Liling, WANG Ke. Determination of 8 Aniline Herbicides in Oil Crops by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(2): 204-209. DOI: 10.13386/j.issn1002-0306.2020040145

超高效液相色谱-串联质谱法测定油料作物中8种苯胺类除草剂

Determination of 8 Aniline Herbicides in Oil Crops by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 建立了玉米、花生等油料作物中8种苯胺类除草剂的超高效液相色谱-串联质谱检测方法。试样经乙腈超声提取后,以N-丙基乙二胺(N-propyl ethylenediamine,PSA)和无水MgSO4净化,ZORBAX Eclipse Plus C18色谱柱(2.1 mm×100 mm,1.8 μm)分离,以甲醇(含1%乙腈)和5 mmol/L乙酸铵水溶液(含0.1%甲酸)为流动相梯度洗脱,流速为0.3 mL/min。采用电喷雾离子源(ESI)正离子模式扫描,多反应监测(MRM)模式进行检测,外标法定量。结果表明,8种苯胺类除草剂在不同浓度范围内(二甲戊乐灵、仲丁灵和磺草唑胺在2.0~200 μg/L,异丙乐灵在5.0~200 μg/L,甲磺乐灵、乙酰甲草胺、氯苯胺灵和氯草灵在0.5~200 μg/L)线性关系良好,相关系数(r)均在0.999以上,在3个不同浓度加标水平下的平均回收率为69.5%~97.5%,相对标准偏差(RSD,n=5)为0.5%~9.5%。方法的检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.07~1.20和0.23~4.00 μg/kg。该方法高效、灵敏,适用于玉米和花生等油料作物中苯胺类除草剂的快速定量检测。

     

    Abstract: A method was developed for the simultaneous determination of 8 aniline herbicides in oil crops by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The samples were ultrasonically extracted with acetonitrile,and then purified with N-propyl ethylenediamine(PSA)and anhydrous magnesium sulfate. The target compounds were separated on a ZORBAX Eclipse Plus C18column(2.1 mm×100 mm,1.8 μm)by gradient elution using methanol(containing 1% acetonitrile)and 5 mmol/L ammonium acetate solution(containing 0.1% formic acid)as mobile phase at a flow rate of 0.3 mL/min. Qualification was achieved by positive electro-spray ionization using multiple reaction monitoring(MRM),and the external standard method was used for quantitation. The calibration curves for 8 aniline herbicides were linear in their corresponding range(2.0~200 μg/L for pendimethalin,butralin and metosulam,5.0~200 μg/L for isopropalin,0.5~200 μg/L for nitralin,diethatyl ethyl,chlorpropham and chlorbufam)with their correlation coefficients(r)all above 0.999. The recoveries for 8 aniline herbicides at three different spiked levels were in the range of 69.5%~97.5% with relative standard deviations(RSD)of 0.5%~9.5%(n=5). The limits of detection(S/N=3)and quantitation(S/N=10)of the method were 0.07~1.20 and 0.23~4.00 μg/kg,respectively. Owing to high efficiency and sensitivity,the method was suitable for rapid and simultaneous analysis of aniline herbicides in oil crops.

     

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