动物性食品中泰妙菌素残留标志物检测UPLC-MS/MS法研究

The Research of 8-α-Hydroxymutilin Residues in Animal Derived Food by UPLC-MS/MS

关键词:  动物性食品  泰妙菌素残留标志物  残留  超高效液相色谱-串联质谱

Key words:  animal derived food  8-α-Hydroxymutilin  residue  UPLC-MS/MS

摘要:

建立了猪和鸡的肌肉、肝脏以及鸡皮+脂组织中泰妙菌素残留标志物(8-α-Hydroxymutilin)残留检测的UPLC-MS/MS方法。样品经酸化丙酮提取，氢氧化钠水解，正己烷除脂，二氯甲烷反萃取后，用C18色谱柱分离，以0.1%甲酸乙腈溶液和0.1%甲酸水溶液为流动相进行梯度洗脱，基质添加标准溶液外标法定量。结果表明：8-α-Hydroxymutilin在20～500 μg/kg猪肌肉、鸡肌肉和鸡皮+脂基质添加标准溶液浓度范围、100～2000 μg/kg猪肝基质添加标准溶液浓度范围、200～4000 μg/kg鸡肝基质添加标准溶液浓度范围内呈现良好线性关系，相关系数R2均大于0.990；方法定量限：猪肌肉、鸡肌肉、鸡皮+脂为25 μg/kg，猪肝脏为100 μg/kg，鸡肝脏为250 μg/kg。猪肌肉、鸡肌肉、鸡皮+脂在25～200 μg/kg添加浓度范围内、鸡肝脏在250～2000 μg/kg添加浓度范围内、猪肝脏在100～1000 μg/kg添加浓度范围内，8-α-Hydroxymutilin的回收率范围均为60%～120%，批内、批间相对标准偏差均小于20％，满足国内外兽药残留相关法规规定。

Abstract:

A UPLC-MS/MS method was established for the determination of 8-α-Hydroxymutilin residue in animal derived food. After extracted by acid acetone and concentrated, the tissues were hydrolyzed by sodium hydrate solution, removed oil by n-hexane. The separation of 8-α-Hydroxymutilin was performed on Waters Acquity UPLC system with the column of BEH C18 and the gradient elution solvent of acetonitrile (0.1% formic acid) and water (0.1% formic acid) at a flow rate of 0.3 mL/min. The method was quantified by blank tissue spiked standard curves. The calibration curves were good linear between the peak areas and the concentrations of 20～500 μg/kg for pig muscle, chicken muscle and skin and fat of chicken，100～2000 μg/kg for pig liver, 200～4000 μg/kg for chicken liver, the correlation coefficient R2＞0.990. The limits of detection of 8-α-Hydroxymutilin in pig muscle, chicken muscle and skin and fat of chicken were 25 μg/kg, in pig liver was 100 μg/kg and in chicken liver was 250 μg/kg. The average recoveries from spiked animal tissues at the concentrations of 25～200 μg/kg for pig muscle, chicken muscle and skin and fat of chicken, 250～2000 μg/kg for chicken liver, 100～1000 μg/kg for pig liver, ranged 60%～120%. The intra- and inter-batch variation coefficients were both less than 20%.