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首页> 外文期刊>Journal of the Brazilian Chemical Society >Validation of a LC-MS/MS Multiresidue Methodology Based on a QuEChERS Approach for the Determination of Fluoroquinolones, Sulfonamides and Trimethoprim in Poultry and Porcine Kidney According to the Normative Instruction 24/2009-MAPA
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Validation of a LC-MS/MS Multiresidue Methodology Based on a QuEChERS Approach for the Determination of Fluoroquinolones, Sulfonamides and Trimethoprim in Poultry and Porcine Kidney According to the Normative Instruction 24/2009-MAPA

机译:基于QuEChERS方法的LC-MS / MS多残留方法学验证,根据规范指示24 / 2009-MAPA测定家禽和猪肾脏中的氟喹诺酮类,磺酰胺类和甲氧苄啶

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摘要

This work involved the validation of a multiresidue method according to the Normative Instruction 24/2009-MAPA for determining 25 analytes, among fluoroquinolones, sulfonamides and trimethoprim in samples of poultry and porcine kidney. The extraction procedure was based on a QuEChERS approach. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed using the selected reaction monitoring mode (SRM) and ESI + ionization. All of the validated figures of merit were evaluated as satisfactory. Accuracy was assessed by recovery studies, varying from 82.7 to 115.5% for porcine kidney and from 91.5 to 110.4% for poultry kidney. Relative standard deviations were lower than 25.5% for porcine kidney, and 29.8% for poultry kidney. Decision limits (CC?±) comprised values from 10.37 to 3298.43 ?μg kg -1 for porcine kidney and 10.08 to 3176.59 ?μg kg -1 for poultry kidney. Detection capabilities (CC?2) varied from 10.73 to 3396.86 ?μg kg -1 for porcine kidney and 10.67 to 3253.19 ?μg kg -1 for poultry kidney. The developed method has been successfully employed in the routine analysis of incurred samples.
机译:这项工作涉及根据规范指令24 / 2009-MAPA验证一种多残留方法的测定方法,该方法用于测定家禽和猪肾脏样品中的氟喹诺酮类,磺酰胺类和甲氧苄啶中的25种分析物。提取程序基于QuEChERS方法。使用选定的反应监测模式(SRM)和ESI +电离,开发了液相色谱-串联质谱(LC-MS / MS)方法。所有经过验证的品质因数均被评估为令人满意。通过恢复研究评估准确性,猪肾脏的准确性从82.7到115.5%,家禽肾脏的准确性从91.5到110.4%。猪肾脏的相对标准偏差低于25.5%,家禽肾脏的相对标准偏差低于29.8%。决定性限值(CC±)的范围为猪肾为10.37至3298.43 µμg kg -1,家禽肾为10.08至3176.59μμgkg -1。猪肾脏的检测能力(CC 2)从10.73到3396.86 µμg kg -1,家禽肾脏的检测能力从10.67到3253.19μμgkg -1。所开发的方法已成功地用于常规样品的分析。

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