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建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定动物源食品中包括19种喹诺酮和11种青霉素在内的30种兽药残留的方法。样品用三氯乙酸乙腈溶液提取,提取液经饱和NaCl溶液和C_(18)分散固相萃取净化后浓缩,正己烷脱脂后测定,以0.2%甲酸水-乙腈作为流动相进行梯度洗脱,在Agilent Eclipseplus C_(18)RRHD(1.8μm,2.1x100 mm)色谱柱上分离,柱温35℃,流速0.3 m L/min,进样量10μL,在电喷雾正离子模式下以动态多反应监测(Dynamic MRM)采集数据,外标法定量。结果表明,30种兽药在相应浓度范围内线性良好,相关系数均大于0.999,不同阴性样品基质中(猪肉、鸡蛋、猪肝)在3个浓度水平加标试验回收率在71.3%~96.5%之间,RSD为2.1%~9.2%,方法检测限(LOD,S/N≥3)为0.5~2.0μg/kg,定量限为2.0~5.0μg/kg。经方法学验证,方法适用于动物源食品中30种兽药残留的快速筛查和定量测定。
A UPLC-MS / MS method was developed for the simultaneous determination of 30 veterinary drug residues in animal-derived foods, including 19 quinolones and 11 penicillins. The sample was extracted with trichloroacetic acid and acetonitrile. The extract was purified by saturated NaCl solution and C 18 disperse solid phase extraction and concentrated. The sample was degreased with n-hexane and eluted with 0.2% formic acid in water as mobile phase. (18 μm) RRHD (1.8 μm, 2.1 × 100 mm) column with a column temperature of 35 ℃ and a flow rate of 0.3 mL / min. The injection volume was 10 μL. The electrospray positive ion mode Dynamic MRM) data acquisition, external standard quantitative. The results showed that the 30 kinds of veterinary drugs had good linearity in the corresponding concentration range, and the correlation coefficients were all greater than 0.999. The recoveries of the spiked samples in three negative samples (pork, egg and pig liver) were 71.3% ~ 96.5% RSD ranged from 2.1% to 9.2%. The limit of detection (LOD, S / N≥3) was 0.5-2.0μg / kg and the limit of quantification was 2.0-5.0μg / kg. The methodological verification, the method is suitable for rapid screening and quantitative determination of 30 veterinary drug residues in animal-derived foods.