QuEChERS-超高效液相色谱串联质谱法测定动物肌肉组织中喹乙醇及卡巴氧代谢物

Determination of olaquindox and carbadox metabolites in animal muscle tissue by QuEChERS-ultra high-performance liquid chromatography-tandem mass spectrometry

中文关键词:  动物肌肉组织  喹乙醇代谢物  卡巴氧代谢物  快速前处理  QuEChERS  超高效液相色谱串联质谱法

英文关键词:animal muscle tissue  metabolite of olaquindox  metabolite of carbadox  rapid pretreatment  QuEChERS  ultra high-performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立QuEChERS-超高效液相色谱串联质谱测定动物肌肉组织中喹乙醇及卡巴氧代谢物的方法。方法 样品经盐酸酸解, 乙酸乙酯提取, 无水硫酸镁和氯化钠盐析, 正己烷除脂净化。经Waters ACQUITY UPLC BEH C18(100 mm×2.1 mm, 1.8 ?m)色谱柱分离, 以0.1%甲酸(A)和0.1%甲酸-甲醇(B)作为流动相, 梯度洗脱。质谱(ESI+)多反应监测(multiple reaction monitoring, MRM), 内标法定量。结果 该方法在1~400 ng/mL浓度范围内线性良好, 相关系数(r2)大于0.99。2种代谢物在0.5、1.0、5.0 μg/kg的添加水平下, 回收率为88.9%~109.2%, 相对标准偏差值在2.18%~8.57%(n=6)。方法检出限为0.5 μg/kg。结论 该方法快速、准确、灵敏, 可用于动物肌肉组织中的喹乙醇及卡巴氧代谢物的快速检测。

英文摘要:

      Objective To establish a method for the detection of olaquindox and carbaxyloxide metabolites in animal muscle tissue by QuEChERS-ultra high-performance liquid chromatography-tandem mass spectrometry. Methods The samples were hydrolyzed by hydrochloric acid, extracted by ethyl acetate, salted out by anhydrous magnesium sulfate and sodium chloride, and fat removed by n-hexane. Separation was carried out on a Waters ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.8 ?m), with 0.1% formic acid (A) and 0.1% formic acid-methanol (B) as mobile phases for gradient elution. Mass spectrometry (ESI +) multiple reaction monitoring (MRM) and internal standard method were used for quantitative analysis. Results The method had good linearity in the concentration range of 1?400 ng/mL, and the correlation coefficient (r2) was greater than 0.99. The recoveries of the 2 metabolites were 88.9%?109.2% and the relative standard deviations were 2.18%?8.57% (n=6) at the addition levels of 0.5, 1.0 and 5.0 μg/kg. The detection limit was 0.5 μg/kg. Conclusion This method is rapid, accurate and sensitive, and can be used for the rapid detection of olaquindox and carbadox metabolites in animal muscle tissue.