超高效液相色谱串联质谱法测定乳制品中 10种青霉素类抗生素残留

Determination of 10 residual penicillin in dairy products by ultra high performance liquid chromatography-tandem mass spectrometry

中文关键词:  青霉素  乳制品  抗生素残留  超高效液相色谱-串联质谱法

英文关键词:penicillin  dairy product  antibiotic residues  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立同时测定乳制品中10种青霉素类抗生素残留的超高效液相色谱-串联质谱分析方法。 方法 样品经乙腈提取后, 乙腈饱和正己烷除去脂肪, 经0.22 μm微孔滤膜过滤, 用乙腈-水(含0.1%甲酸5 mmol/L乙酸铵)为流动相, C18柱分离, 20 min内梯度洗脱分离10种青霉素; 电喷雾正离子模式电离(ESI+), 多反应监测模式检测(MRM), 外标法定量。结果 在0.1~20 μg/L浓度范围内, 10种青霉素类药物在各种乳制品基质中均有良好的线性关系, 线性相关系数均＞0.999; 液体乳最低检测限为0.2 μg/kg~1.0 μg/kg, 乳粉的最低检测限1.0 μg/kg~5.0 μg/kg; 方法回收率在70.2%~108.2%, 相对标准差为＜15%。结论 该方法测定乳制品中10种青霉素药物的残留量简便、快速、准确, 可以满足对青霉素类抗生素的监测要求。

英文摘要:

      Objective To establish a method for simultaneous determination of 10 residual penicillin in dairy products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted with acetonitrile and degreased with saturated acetonitrile n-hexane and filtered through 0.22 μm millipore membrane. The filtrate was detected by ultra high performance liquid chro-matography-tandem mass spectrometry, identified by electrospray ionization (ESI) in positive mode using multiple reactions monitoring mode, and quantified with external standard method. The sample extract was separated on a C18 column by gradient elution in 20 min with acetronitrile-water (containing 0.1% formic acid and 5 mmol/L ammonium acetate) as mobile phase. Results The calibration curve of the 10 penicillins residues showed a good linearity in the range of 0.1 μg/L~20.0 μg/L in various dairy products in the matrix with the correlation coefficient r2>0.999. The detection limit of the method was 0.2 μg/kg~1.0 μg/kg for liquid milk and 1.0 μg/kg~5.0 μg/kg for milk powder. The recoveries of spiking levels ranged from 70.2% to 108.2%, and the relative standard deviation (RSD) was less than 15%. Conclusion The method for determination of residues of 10 penicillin antibiotics in dairy products is simple, rapid and accurate, and could satisfy the requirements for monitoring of penicillin residues