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首页> 外文期刊>Meat Science >Development of QuEChERS-based extraction and liquid chromatography-tandem mass spectrometry method for quantifying flumethasone residues in beef muscle
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Development of QuEChERS-based extraction and liquid chromatography-tandem mass spectrometry method for quantifying flumethasone residues in beef muscle

机译:基于QuEChERS的萃取和液相色谱-串联质谱法定量分析牛肉肌肉中的氟甲米松残留量

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摘要

A rapid, specific, and sensitive method based on liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM) was developed and validated to quantify flumethasone residues in beef muscle. Methods were compared between the original as well as the EN quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based extraction. Good linearity was achieved at concentration levels of 5-30 μg/kg. Estimated recovery rates at spiking levels of 5 and 10 ug/kg ranged from 72.1 to 84.6%, with relative standard deviations (RSDs)<7%. The results of the inter-day study, which was performed by fortifying beef muscle samples (n= 18) on 3 separate days, showed an accuracy of 93.4-94.4%. The precision (expressed as relative standard deviation values) for the inter-day variation at two levels of fortification (10 and 20 μg/kg) was 1.9-5.2%. The limit of detection (LOD) and limit of quantitation (LOQ) were 1.7 and 5 μg/kg, at signal-to-noise ratios (S/Ns) of 3 and 10, respectively. The method was successfully applied to analyze real samples obtained from large markets throughout the Korean Peninsula. The method proved to be sensitive and reliable and, thus, rendered an appropriate means for residue analysis studies.
机译:建立了一种基于正离子模式的液相色谱-电喷雾串联质谱法(LC-ESI-MS / MS)的快速,特异性和灵敏的方法,并使用多反应监测(MRM)进行了验证,该方法可定量分析牛肉肌肉中的氟美松酮残留量。在原始方法以及基于EN的快速,简便,廉价,有效,坚固和安全(QuEChERS)提取方法之间进行了比较。在5-30μg/ kg的浓度水平下实现了良好的线性。加标水平为5和10 ug / kg时,估计的回收率在72.1至84.6%之间,相对标准偏差(RSD)<7%。通过在3天中强化牛肉肌肉样本(n = 18)进行的日间研究的结果显示,准确度为93.4-94.4%。在两个设防水平(10和20μg/ kg)下,日间变化的精度(表示为相对标准偏差值)为1.9-5.2%。当信噪比(S / Ns)分别为3和10时,检测限(LOD)和定量限(LOQ)分别为1.7和5μg/ kg。该方法已成功应用于分析从整个朝鲜半岛的大型市场获得的真实样品。该方法被证明是灵敏和可靠的,因此为残留物分析研究提供了一种合适的方法。

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  • 来源
    《Meat Science》 |2012年第4期|p.749-753|共5页
  • 作者单位

    Natural Products Chemistry Laboratory, Biotechnology Research Institute, Chonnam National University, 77 Yongbong-ro, Buk-gu, Gwangju 500-757, Republic of Korea;

    Institute of Environmental Research (INFU), Faculty of Chemistry, TU Dortmund University, Otto-Hahn Str. 6, Campus North, D-44227 Dortmund, Germany;

    Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, 12211-Giza, Egypt;

    National Agricultural Products Quality Management Service, Products Safety Inspection Laboratory, Gwangsan-Gu, Gwangju, Republic of Korea;

    Natural Products Chemistry Laboratory, Biotechnology Research Institute, Chonnam National University, 77 Yongbong-ro, Buk-gu, Gwangju 500-757, Republic of Korea;

    Korea Food & Drug Administration, Food Chemical Residues Division, Osong Health Technology Administration Complex, 187 Osongsaengmyeong2(i)-ro, Osong-eup, Cheongwon-gun, Chungcheongbuk-do, Republic of Korea;

    Korea Food & Drug Administration, Food Chemical Residues Division, Osong Health Technology Administration Complex, 187 Osongsaengmyeong2(i)-ro, Osong-eup, Cheongwon-gun, Chungcheongbuk-do, Republic of Korea;

    Korea Food & Drug Administration, Food Chemical Residues Division, Osong Health Technology Administration Complex, 187 Osongsaengmyeong2(i)-ro, Osong-eup, Cheongwon-gun, Chungcheongbuk-do, Republic of Korea;

    Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, ! Hwayang-dong, Kwangjin-gu, Seoul 143-701, Republic of Korea;

    Regional FDA Hazardous Substances Analysis Division, Daejeon, Republic of Korea;

    Natural Products Chemistry Laboratory, Biotechnology Research Institute, Chonnam National University, 77 Yongbong-ro, Buk-gu, Gwangju 500-757, Republic of Korea;

  • 收录信息 美国《科学引文索引》(SCI);
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

    corticosteroids; flumethasone; residue analysis; LC-MS/MS; beef muscles;

    机译:皮质类固醇;氟米松残留分析LC-MS / MS;牛肉肌肉;

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