超高效液相色谱-串联质谱法检测牛肉中16种镇静剂类药物残留
目的 建立超高效液相色谱-串联质谱法测定牛肉中镇静剂类药物代谢物残留的方法。方法 采用对样品碱水解, Oasis MCX阳离子固相萃取小柱净化后, 超高效液相色谱-串联质谱多反应监测(multiple reaction monitoring, MRM)模式测定。色谱柱: AQUITY UPLC BEH C18(100 mm×2.1 mm, 1.7 μm); 柱温: 40 ℃; 样品室温度: 4 ℃; 流动相: A相为酸化乙腈, B相为0.1%甲酸水, 梯度洗脱; 流速: 0.3 mL/min; 进样体积: 10 μL。 结果 0.1~20.0 μg/L范围内16种镇静剂的浓度与色谱峰面积响应之间线性关系良好(r≥0.995)。最低检出限为0.03~0.7 μg/kg。平均回收率为89.7%~114.0%, RSD为0.4%~16.9%。结论 本方法检出限低, 精密度高, 适用于牛肉中镇静剂类药物残留的检测。
Objective To establish a method for the determination of 16 sedative residues in beef by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was hydrolyzed by alkali, Oasis MCX cationic solid phase extraction column was purified and determined by HPLC-MS with multiple reaction monitoring mode. Chromatographic column was AQUITY UPLC BEH C18 (100 mm×2.1 mm, 1.7 μm), column temperature was 40 ℃, sample temperature was 4 ℃, mobile phase was gradient elution solvent, with the mobile phase of A phase of acetonitrile acidification, and B phase of 0.1% formic acid water. Flow rate was 0.3 mL/min, and injection volume was 10 μL. Results The 16 pesticides had good linear relationships in the range of 0.1-20.0 μg/L, and the correlation coefficients were larger than or equal to 0.995. The limits of detection (LODs) were 0.03-0.7 μg/kg. The recoveries were 89.7%-114.0%, with the relative standard deviations (RSD) of 0.4%-16.9%.Conclusion The method has low limit of detection, and high precision, which is suitable for determination of sedative residues in beef.
标题：超高效液相色谱-串联质谱法检测牛肉中16种镇静剂类药物残留
英文标题：Determination of 16 sedative residues in beef by ultra high performance liquid chromatography-tandem mass spectrometry
作者：
冯静 辽宁省疾病预防控制中心
邹淼 辽宁省疾病预防控制中心
陈曦 辽宁省疾病预防控制中心
祁珍祯 辽宁省疾病预防控制中心
华正罡 辽宁省疾病预防控制中心
中文关键词:超高效液相色谱-串联质谱法,牛肉,畜肉,镇静剂类药物残留,
英文关键词:ultra high performance liquid chromatography-tandem mass spectrometry,beef,livestock products,sedative drug residues,
发表日期：2019-01-31
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