高效液相色谱-四极杆轨道阱高分辨质谱对动物源食品中抗生素类成分的快速筛查

Screening of antibiotics in foodstuffs of animal origin by high performance liquid chromatography-quadrurpole/electrostatic field orbitrap high resolution mass spectrometry

目的建立动物源食品中抗生素快速筛查的Q-Exactive方法。方法采用酸性乙腈提取动物源食品中的抗生素类化合物,QuEChERS净化,乙腈水定容,ACQUITY BEH C18色谱柱分离,以0.1%甲酸-乙腈为流动相,梯度洗脱分离。Q-Exactive一级全扫描得到的准分子离子的精确质量数用于快速筛选分析,保留时间和离子阱的二级质谱数据用于进一步定性确证。结果 31种抗生素的精确质量相对偏差小于5×10-6,线性相关系数均大于0.99,最低检出限(limit of detection,LOD)均≤10μg/kg。结论应用该方法对鱼、牛奶、蜂蜜等实际样品筛查的分析结果良好,说明该方法是动物源食品中抗生素类成分快速筛选和确证的有效方法。

Objective Todevelop a method of high performance liquid chromatography (HPLC) coupled with linear ion trap/Orbitrap high resolution mass spectrometry (QuEChERS) to detect antibiotics quickly in food of animal origin.Methods Antibiotics in samples were extracted using a solvent of acidic acetonitrile, following by purification with QuEChERS, dilution with acetonitrile and H2O. The separation was performed on an ACQUITY BEH C18column using gradient elution with aqueous solution (containing 0.1% formic acid)/acetonitrile as a mobile phase. The accurate mass of quasi-molecular ion were acquired by full scanning of electrostatic field orbitrap and applied for rapid screening and analysis, further confirmation was accomplished according to the retention time and qualitative fragments obtained by data dependent scan mode. ResultsUnder the optimal conditions, 31 antibiotics were routinely detected with mass accuracy error below 5×10―6, and good linearity were provided in their respective linear ranges with correlation coefficients all higher than 0.99, the limit of detection (LOD) for all the 31 antibiotics were≤10μg/kg. ConclusionThe method was applied to fish, milk, and honey and satisfying screening results proved that it is an efficient path for rapid analysis of antibiotics in food of animal origin.