应用PRiME HLB净化技术,采用超高效液相色谱-串联四级杆质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)分析手段,建立动物源性食品中12种青霉素族抗生素类药物残留量的检测方法。该文着重对样品的净化、浓缩、液相分离及串联质谱等相关检测参数进行了最佳化研究。样品经80%乙腈水混合溶液提取,PRiME HLB固相萃取柱净化,经CORTECS C18色谱柱(100 mm×2.1 mm,2.7 μm),以甲醇和0.1%甲酸水溶液为流动相梯度洗脱,以MRM方式进行定量分析。结果表明,各组分在各自浓度范围内线性关系良好,相关系数r2≥0.998,平均回收率在81.7%~111.9%,相对标准偏差在0.89%~8.56%。该方法用于食品中青霉素族抗生素药物残留检测,具有准确、快速、简便、灵敏度高等优点,可满足我国对青霉素族抗生素类药物检测限要求。
PRiME HLB purification technique was used to determine the residues of 12 penicillin antibiotics in food by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).In this study, the optimum parameters of purification, concentration, liquid phase separation and tandem mass spectrometry were optimized.The samples were extracted by 80% acetonitrile water mixed solution, purified by PRiME HLB, and separated by CORTECS C18 column (100 mm×2.1 mm, 2.7 μm) with methanol and 0.1% formic acid solution as the mobile phase gradient elution and MRM quantitative analysis.The results showed that each component had a good linear relationship with correlation coefficient R2≥0.998, the average recovery rate was 81.7%-111.9% and the relative standard deviation was 1.82%-8.56%.This method can be used for the determination of penicillin family antibiotics in food.It has the advantages of accuracy, simplicity, sensitivity and high sensitivity.It meets the requirements for the detection of penicillin and antibiotics in China.