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首页> 外文期刊>The Journal of automatic chemistry >A Convenient and Sensitive LC-MS/MS Method for Simultaneous Determination of Carbadox- and Olaquindox-Related Residues in Swine Muscle and Liver Tissues
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A Convenient and Sensitive LC-MS/MS Method for Simultaneous Determination of Carbadox- and Olaquindox-Related Residues in Swine Muscle and Liver Tissues

机译：一种同时灵敏的LC-MS / MS方法，可同时测定猪肌肉和肝组织中卡巴多克斯和奥拉喹酮的残留量

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This paper presents a convenient and sensitive LC-MS/MS method for the simultaneous determination of carbadox and olaquindox residues, including desoxyolaquindox (DOLQ), desoxycarbadox (DCBX), quinoxaline-2-carboxylic acid (QCA), 3-methyl-quinoxaline-2-carboxylic acid (MQCA), and the glycine conjugates of QCA and MQCA (namely, QCA-glycine and MQCA-glycine, resp.) in swine muscle and liver tissues. Tissue samples were extracted with 2% metaphosphoric acid in 20% methanol and cleaned up by solid-phase extraction (SPE) on a mixed-mode anion-exchange column (Oasis MAX). Analysis was performed on a C18 column by detection with mass spectrometry in the multiple reaction monitoring (MRM) mode. The limits of detection (LODs) of the six analytes were determined to be 0.01?μg·kg?1 to 0.25?μg·kg?1, and the limits of quantification (LOQs) were 0.02?μg·kg?1 to 0.5?μg·kg?1. The total recoveries of the six analytes in all tissues were higher than 79.1% with the RSD% less than 9.2%. The developed method can determine the real residue level of QCA and MQCA, whether they are present in free form or as glycine conjugates in tissues, together with the carcinogenic desoxy metabolites DCBX and DOLQ with high recovery. Therefore, this method was suitable for routine analysis of residue control programmes and the residue depletion study of CBX and OLQ on swine.
机译：本文提出了一种简便而灵敏的LC-MS / MS方法，可同时测定卡巴多斯和olaquindox残留物，包括去氧喹啉（DOLQ），去氧卡多氧（DCBX），喹喔啉-2-羧酸（QCA），3-甲基喹喔啉- 2-羧酸（MQCA），以及猪肌肉和肝组织中QCA和MQCA的甘氨酸共轭物（即QCA-甘氨酸和MQCA-甘氨酸，分别）。组织样品用2％偏磷酸的20％甲醇溶液萃取，并通过固相萃取（SPE）在混合模式阴离子交换柱（Oasis MAX）上进行纯化。通过在多反应监测（MRM）模式下用质谱检测对C18色谱柱进行分析。六个分析物的检出限（LOD）为0.01？μg·kg？1至0.25？μg·kg？1，定量限（LOQs）为0.02？μg·kg？1至0.5？ μg·kg？1。所有组织中六种分析物的总回收率均高于79.1％，RSD％低于9.2％。所开发的方法可以测定QCA和MQCA的真实残留水平，无论它们以游离形式存在还是以甘氨酸缀合物形式存在于组织中，并具有高回收率的致癌脱氧代谢产物DCBX和DOLQ。因此，该方法适用于残留控制程序的常规分析以及猪中CBX和OLQ的残留消耗研究。

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