超高效液相色谱串联质谱法同时检测蜂蜜中多种抗生素残留的研究

旨在建立一种同时测定蜂蜜中多种抗生素残留的超高效液相色谱串联质谱检测方法。样品经1%甲酸乙腈-Na2EDTA水溶液提取后,盐析除水,于上清液中加入C18吸附剂净化,取上清液浓缩复溶后,过膜待测。采用C18色谱柱(2.1mm×100mm,1.7μm)分离,以0.1%甲酸水溶液和甲醇溶液作为流动相进行梯度洗脱,超高效液相色谱串联质谱法(UPLC-MS/MS)同时定性、定量测定蜂蜜中多种抗生素残留。结果表明,待测药物在0.01~5.00μg/mL检测范围内线性关系良好,相关系数(r)均在0.99以上;在1、5、10μg/kg3个浓度水平上进行添加回收实验,平均回收率为68.0%~104.0%,相对标准偏差为3.2%~15.5%,方法的检出限可以达到1μg/kg。该方法重现性好、灵敏度高、分析时间短、确证能力强,适用于蜂蜜中多种抗生素残留的同时检测。

Simultaneous Determination of Multiple Antibiotics in Honey by UPLC-MS/MS

A method for simultaneous determination of multiple antibiotic residues in honey was developed by means of a series mass spectrometry(MS)methods.After the sample was extracted from 1%acetonitrile formate-Na2EDTA aqueous solution,the containing salt was removed from the water,and the C18 adsorbent was added to the upper liquid to purify it.After concentrated and dissolved,the solution was filtered by a membrane filter.The prepared samples were separated by the C18 chromatographic column(2.1 mm×100 mm,1.7μm),and 0.1%formic acid aqueous solution and methanol solution were used as the flow phase for gradient elution.The UPLC-MS/MS method was used to qualitatively and quantitatively determine multiple antibiotic residues in honey simultaneously.The results showed that the linear relationship of the drugs to be tested was good in the range of 0.01μg/mL to 5.00μg/mL,and the correlation coefficient(r)was all above 0.99.Addition recovery experiments were conducted at 1,5 and 10μg/kg concentration levels,the average recovery rate was between 68.0%and 104.0%,and the relative standard deviation ranged from 3.2% to 15.5%.The detection limit of the developed method reached up to 1μg/kg.The method has good reproducibility,high sensitivity,short analysis time and strong corroboration ability,which is recommended to be used in simultaneous determination of multiple antibiotics residues in honey.