Zhang Heying, Qu Wei, Tao Yanfei, Chen Dongmei, Xie Shuyu, Huang Lingli, Liu Zhenli, Pan Yuanhu, Yuan Zonghui
MOA Laboratory for Risk Assessment of Quality and Safety of Livestock and Poultry Products, Huazhong Agricultural University, Wuhan, Hubei 430070, China.
National Reference Laboratory of Veterinary Drug Residues and MAO Key Laboratory for Detection of Veterinary Drug Residues, Huazhong Agricultural University, Wuhan, Hubei 430070, China.
J Anal Methods Chem. 2018 Jun 14;2018:2834049. doi: 10.1155/2018/2834049. eCollection 2018.
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 C 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 g·kg to 0.25 g·kg, and the limits of quantification (LOQs) were 0.02 g·kg to 0.5 g·kg. 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.
本文介绍了一种简便、灵敏的液相色谱-串联质谱法，用于同时测定猪肌肉和肝脏组织中卡巴多司和喹乙醇残留，包括脱氧喹乙醇（DOLQ）、脱氧卡巴多司（DCBX）、喹喔啉-2-羧酸（QCA）、3-甲基喹喔啉-2-羧酸（MQCA）以及QCA和MQCA的甘氨酸缀合物（分别为QCA-甘氨酸和MQCA-甘氨酸）。组织样品用20%甲醇中的2%偏磷酸提取，并通过混合模式阴离子交换柱（Oasis MAX）上的固相萃取（SPE）进行净化。在C柱上进行分析，采用多反应监测（MRM）模式的质谱检测。六种分析物的检测限（LOD）为0.01 g·kg至0.25 g·kg，定量限（LOQ）为0.02 g·kg至0.5 g·kg。所有组织中六种分析物的总回收率均高于79.1%，相对标准偏差（RSD%）小于9.2%。所建立的方法能够测定组织中以游离形式或甘氨酸缀合物形式存在的QCA和MQCA的实际残留水平，以及具有致癌性的脱氧代谢产物DCBX和DOLQ，回收率高。因此，该方法适用于残留控制计划的常规分析以及CBX和OLQ在猪体内的残留消除研究。
