液相色谱-串联质谱法快速测定鸡蛋中金刚烷胺、氟苯尼考和氟苯尼考胺残留量
目的 建立同时测定鸡蛋中金刚烷胺、氟苯尼考及氟苯尼考代谢物氟苯尼考胺残留的液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS)快速分析方法。方法 鸡蛋样品用1.0%乙酸乙腈提取, 提取后用PSA和C18净化, 氮吹后用流动相复溶, 复溶液过滤膜后进行液相色谱-串联质谱测定。分析采用XBridge C18色谱柱, 以0.02%甲酸溶液和甲醇乙腈混合溶剂为流动相进行梯度洗脱, 正负离子切换监测模式下进行监测, 同位素内标法定量。结果 3种化合物在一定浓度(氟苯尼考为0.10~20 μg/L, 金刚烷胺和氟苯尼考胺为0.5~100 μg/L)范围内具有较好的线性关系, 金刚烷胺、氟苯尼考和氟苯尼考胺的检出限(limit of detection, LOD)分别为0.3、0.06、0.3 μg/kg, 定量限(limit of quantitation, LOQ)分别为1.0、0.20、1.0 μg/kg。当3种化合物在鸡蛋中的加标水平为LOQ、5LOQ和10LOQ时, 平均回收率在94.9%~102%之间, 相对标准偏差范围为1.2%~4.9%。结论 方法简便、快速、准确, 能满足鸡蛋中金刚烷胺和氟苯尼考残留量同时分析需要。
Objective To establish a rapid method for simultaneous determination of amantadine, florfenicol and florfenicol amine residues in eggs by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Egg samples were extracted with 1.0% acetonitrile acetate, purified with PSA and C18, and dissolved with mobile phase after nitrogen blowing, detected by LC-MS/MS after filtering the solution. An XBridge C18 column was used for the separation by gradient elution using a mixture of 0.02% formic acid solution and methanol/acetonitrile as the mobile phase, and a mass spectrometer was used in the positive and negative ion mode. The samples were quantified with the isotope dilution and internal standard methods. Results Three compounds had good linear relationships in the range of 0.10?20 μg/L (florfenicol) or 0.50?100 μg/L (amantadine and florfenicol amine). The limits of detection of amantadine, florfenicol and florfenicol amine were 0.30, 0.06, and 0.30 μg/kg, respectively. The limits of quantitation of amantadine, florfenicol and florfenicol amine were 1.0, 0.20, and 1.0 μg/kg, respectively. The recoveries at 3 spiked levels (LOQ, 5LOQ, 10LOQ) were 94.9%?102%, with the relative standard deviations of 1.2%?4.9%. Conclusion This method is simple, rapid and accurate, which is suitable for simultaneous determination of amantadine, florfenicol and florfenicol residues in eggs.
标题：液相色谱-串联质谱法快速测定鸡蛋中金刚烷胺、氟苯尼考和氟苯尼考胺残留量
英文标题：Rapid and simultaneous determination of amantadine, florfenicol and florfenicol amine residues in eggs by liquid chromatography-tandem mass spectrometry
作者：
陈国 宁波市农业科学研究院
王全胜 宁波市农业科学研究院
吴银良 宁波市农业科学研究院
中文关键词:金刚烷胺,氟苯尼考,鸡蛋,液相色谱-串联质谱法,残留,
英文关键词:amantadine,florfenicol,eggs,liquid chromatography-tandem mass spectrometry,residues,
发表日期：2019-02-15
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