超高效液相色谱-串联质谱法检测饲料中喹烯酮和喹乙醇

Detection of quicetone and olaquindox in feedstuff by UPLC-MS-MS

本文应用超高效液相色谱-串联质谱技术,建立了饲料中喹烯酮和喹乙醇的检测方法。样品经0.1%甲酸乙腈溶液提取后,通过PRiME HLB固相萃取柱净化;采用0.1%甲酸乙腈溶液作为流动相进行梯度洗脱,经AtlantisT3色谱柱分离,通过多反应监测模式进行测定。在5～500 ng/mL时线性关系良好,相关系数均大于0.996。在0.2、0.4、2 mg/kg添加水平下,平均回收率为80%～95.5%,相对标准偏差均小于10%。检测限为0.06 mg/kg,定量限为0.2 mg/kg,该法准确、简单、快速。

A method of Ultra-HPLC-MS/MS was developed to determine quicetone and olaquindox in feedstuff.The samples were extracted by 0.1%formic acid acetate solution and separated by a PRiME HLB cation exchange chromatographic column.The HPLC separation was performed on Atlantis T3 column with a linear gradient elution program of 0.1%formic aci formate solution as the mobile phase.Selective reaction monitoring was used for the selective detection.There was a good line correlation in the range of 5~500 ng/mL,the correlation coefficient was greater than 0.996.The average recorvery was 80%~95.5%and RSD were both less than 10%.The limit of detection was 0.06 mg/kg and limit of quantification was 0.2 mg/kg.The method was accurate,convenient and fast.