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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0.22μm微孔滤膜过滤,用乙腈-水(含0.1%甲酸5mmol/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0.1~20μg/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0.2μg/kg~1.0μg/kg,乳粉的最低检测限1.0μg/kg~5.0μg/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。
OBJECTIVE To establish a method for the simultaneous determination of 10 penicillin antibiotics residues in dairy products by ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile and saturated with hexane to remove fat, filtered through 0.22μm microporous membrane, and separated on a C18 column with acetonitrile-water (5mmol / L ammonium acetate containing 0.1% formic acid) Elution and separation of 10 kinds of penicillin; electrospray positive ionization mode (ESI +), multiple reaction monitoring mode (MRM), external standard method. Results In the concentration range of 0.1 ~ 20μg / L, 10 kinds of penicillins showed good linearity in all kinds of dairy matrices with linear correlation coefficients> 0.999. The detection limit of liquid milk was 0.2μg / kg ~ 1.0μg / kg, and the detection limit of milk powder was 1.0μg / kg ~ 5.0μg / kg. The recovery rate was 70.2% -108.2% with the relative standard deviation of <15%. Conclusion The method of determination of 10 kinds of penicillin residues in dairy products is simple, rapid and accurate, and can meet the monitoring requirements of penicillin antibiotics.