高效液相色谱-串联质谱法同时测定动物源性食品中35种兽药残留量
Simultaneous HPLC-MS/MS Determination of 35 Veterinary Drugs in Animal Derived Food
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摘要: 提出了高效液相色谱-串联质谱法同时测定动物源性食品中35种兽药残留量的方法。样品经含1%(体积分数)乙酸的乙腈提取,QuEChERS方法净化,所得净化液以Zobax Eclipse Plus C18色谱柱为分离柱,以不同体积比的0.1%甲酸(体积分数)溶液和乙腈混合液为流动相进行梯度洗脱,采用电喷雾正离子源和多反应监测模式检测。35种化合物的质量分数均在1~50 μg·kg-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.02~1.07 μg·kg-1之间,测定下限(10S/N)在0.08~3.58 μg·kg-1之间。以空白样品为基体进行加标回收试验,所得回收率在45.6%~121%之间,相对标准偏差(n=6)在2.4%~24%之间。Abstract: A method of HPLC-MS/MS for the simultaneous determination of 35 veterinary drugs in food of animal origin was proposed. The sample was extracted with acetonitrile (containing 1% by vol. of acetic acid) and purified by the QuEChERS method. Zobax Eclipse Plus C18 column was used as stationary phase in chromatographic separation, and the mixture of 0.1% (φ) formic acid solution and acetonitrile mixed in different ratio was used as mobile phase in gradient elution. ESI+ and multi-reaction monitoring were adopted in MS/MS. Linear relationships between values of peak area and mass fraction of the 35 compounds were kept in the same range of 1-50 μg·kg-1, with detection limits (3S/N) in the range of 0.02-1.07 μg·kg-1 and lower limits of determination (10S/N) in the range of 0.08-3.58 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 45.6%-121%, with RSD′s (n=6) in the range of 2.4%-24%.