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

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20~500μg/kg猪肌肉、鸡肌肉和鸡皮+脂基质添加标准溶液浓度范围、100~2000μg/kg猪肝基质添加标准溶液浓度范围、200~4000μg/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R^2均大于0.990;方法定量限:猪肌肉、鸡肌肉、鸡皮+脂为25μg/kg,猪肝脏为100μg/kg,鸡肝脏为250μg/kg。猪肌肉、鸡肌肉、鸡皮+脂在25~200μg/kg添加浓度范围内、鸡肝脏在250~2000μg/kg添加浓度范围内、猪肝脏在100~1000μg/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。

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 Acquity UPLC system with the column of BEH C18 and the of 8 -α -Hydroxymutilin was performed on Waters 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 txg/kg for pig muscle, chicken muscle and skin and fat of chicken, 100 -2000 μg/kg for pig liver, 200 - 4000μg/kg for chicken liver, the correlation coefficient R^2 〉 0. 990. The limits of detection of 8 -α- Hydroxymutilin in pig muscle, was 100 p.g/kg and in chicken liver w concentrations of 25 ～ 200μg/kg for pig for chicken liver, 100 - 1000 μg/kg fo coefficients were both less than 20%. chicken muscle and skin and fat of chicken were 25 iμg/kg, in pig liver as 250 μg/kg. The average recoveries from spiked animal tissues at the g muscle, chicken muscle and skin and fat of chicken, 250～ 2000 μg/kg r pig liver, ranged 60% - 120%. The intra - and inter - batch variation coefficients were both less than 20%.