目的: 建立固相萃取-超高效液相色谱串联三重四极杆质谱法（UPLC-QQQ MS/MS法）测定中药鸡内金中68种兽药残留。方法: 样品匀质后,经乙腈和含0.5%甲酸的乙腈进行2次提取,并经Oasis PRiME HLB固相萃取柱净化。采用Agilent ZORBAX Eclipse Plus C18（3.0 mm×150 mm,1.8 μm）色谱柱分离,以乙腈和5 mmol · L-1乙酸铵水溶液（含0.1%甲酸）体系为流动相进行梯度洗脱;ESI电离源,正、负离子模式,多反应监测（MRM）,空白基质匹配标准曲线法定量。结果: 68种兽药在一定质量浓度范围内线性关系良好,r≥0.995 8;方法检测限（LOD）为0.1~3 μg · kg-1,定量限（LOQ）为0.2~10 μg · kg-1;3个浓度水平下（n=6）加样回收率在61.9%~121.5%,RSD为0.50%~8.4%。在50批鸡内金样品中共有5批检出兽药残留,检出的兽药残留包括金刚烷胺、多西环素、恩诺沙星、氟苯尼考。结论: 本方法简便、快捷、准确、可靠,适用于鸡内金中多种兽药残留的测定。
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