| 超高效液相色谱-串联质谱法测定苹果和土壤中乙嘧酚残留量 |
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| 引用本文： | 梁京芸,李增梅,郭长英,刘俊华,苑学霞,刘美.超高效液相色谱-串联质谱法测定苹果和土壤中乙嘧酚残留量[J].山东农业科学,2013,45(4):101-104,108. |
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| 作者姓名： | 梁京芸 李增梅 郭长英 刘俊华 苑学霞 刘美 |
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| 作者单位： | 1. 山东省农业科学院农业质量标准与检测技术研究所/山东省食品质量与安全检测技术重点实验室,山东济南,250100
2. 山东农业大学动物科技学院,山东泰安,271018 |
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| 基金项目： | 山东省科学仪器设备升级改造技术研究专项 |
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| 摘 要： | 建立了苹果和土壤中超高效液相色谱-串联质谱法(UPLC-MS/MS)检测乙嘧酚残留方法,考察了基质效应,并对实际样品进行了检测。苹果和土壤经乙腈振荡提取后,用MCX柱净化,采用UPLC-MS/MS正离子扫描分析乙嘧酚。以苹果和土壤为基质进行3档添加水平和5次重复性试验,结果表明添加浓度为0.01、0.05、0.1 mg/kg的平均回收率为88%～102%,相对标准偏差为2.1%～8.7%。本方法在苹果和土壤中的检出限为2μg/kg,定量限为4μg/kg,在10～300μg/L范围内线性关系好(r>0.999)。
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| 关 键 词： | 乙嘧酚 超高效液相色谱-串联质谱 残留 苹果 土壤 |
Determination of Ethirimol Residue in Apple and Soil by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| Liang JingYun
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Li ZengMei
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Guo ChangYing
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Liu JunHua
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Yuan XueXia
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Liu Mei.Determination of Ethirimol Residue in Apple and Soil by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Shandong Agricultural Sciences,2013,45(4):101-104,108. |
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| Authors: | Liang JingYun Li ZengMei Guo ChangYing Liu JunHua Yuan XueXia Liu Mei |
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| Institution: | 1. Institute of Agricultural Quality Standard and Testing Technology, Shandong Academy of Agricultural Sciences, Jiuan 250100, China ; 2. College of Animal Science, Shandong Agricultural University, Taian 271018, China) |
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| Abstract: | A new method for the confirmation and quantification of ethirimol residues in apple and soilwas established based on ultra performance liquid chromatography- tandem mass spectrometry. The matrixeffects for the method were also studied. The apple and soil were extracted with acetonitrile by an oscillator,and purified with MCX column. The detection was performed by tandem mass spectrometry with electrospray i-onization in positive mode （ESI ＋ ）. The average recoveries of ethirimol at three spiked levels （0.01,0.05,0.1mg/kg） in apple and soil were found as 88% - 102% with the RSD as 2.1%-8.7%. The limit of detec-tion （LOD） of ethirimol in apple and soil was 2 μg/kg, and the limit of quantitation was 4 μg/kg. A goodlinear relationship was obtained in the range of 10 - 300μg/L with the correlation coefficient over 0. 999. |
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| Keywords: | Ethirimol Ultra performance liquid chromatography -tandem mass spectrometry Residue Apple Soil |
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