UPLC-MS/MS测定牛奶中9种青霉素

Simultaneous Determination of Nine Penicillin Residues in Milk by UPLC-MS/MS

建立超高效液相色谱-串联四极杆质谱多反应离子监测模式同时测定牛奶中9种青霉素类抗生素(包括羟氨苄青霉素、氨苄青霉素、邻氯青霉素、双氯青霉素、乙氧柰胺青霉素、苯唑青霉素、苄青霉素、苯氧甲基青霉素、甲氧苯基青霉素)残留量的检测方法。样品采用乙腈沉淀蛋白、脱脂后,过HLB小柱净化、富集。以0.01 mol/L乙酸铵水(甲酸调节p H 4.5)-乙腈梯度洗脱,经Agilent Eclipse plus C18色谱柱(2.1×100 mm,粒径1.8μm)分离后,采用MRM模式进行定量定性分析。结果:结果表明9种抗生素在0.1μg/L^100μg/L范围内线性关系良好,高中低浓度回收率在67.7%~92.8%,相对标准偏差(n=6)小于15%,各组分定量限为0.1μg/kg^4μg/kg。

A ultra performance liquid chromatography tandem quadrupole mass spectrometry method was devel- oped for the analysis of nine penicillin residues （amoxicillin, ampicillin, cloxacillin, dieloxacillin, nafcillin, oxacillin, gpenicillin, penicillin, methicillin） in milk, simutaneously. Protein and fat in the samples were re- moved by acetonitrilc and n-hexane respectively, then the samples were purified on HLB column and concen- trated under N2. The analytes were separated on an Agilent Eclipse plus C18 column （2.1x100 mm,dpl.8 μm） with gradient elution consisted of 0.01 mol/L ammonium acetate （pH4.5） and acetonitrile, and analyzed under the mode of MRM. The results showed good linearity in the ranges of 0.1 μg/L-100 μg/L. The recoveries were between 67.7 % and 92.8 %, and the values of the RSD （n=6） were lower than 15 % for all the analytes. The limits of quantitatitation （LOQ） for the analytes range from 0.1 μg/kg to 4 p,g/kg. The method was suitable to de- tect penicillins in milk simultaneously with good accuracy and reputability.