液相色谱-四极杆-静电场轨道阱高分辨质谱法测定牛奶中8种氨基糖苷类抗生素残留

Determination of Eight Aminoglycoside Residues in Milk by Liquid Chromatography- Quadrupole-Orbitrap High Resolution Mass Spectrometry

建立了一种测定牛奶中链霉素、双氢链霉素、庆大霉素、大观霉素、新霉素、卡那霉素、阿米卡星和安普霉素8种氨基糖苷类药物的液相色谱-四极杆-静电场轨道阱高分辨质谱方法。样品经提取和分子印迹固相萃取柱净化,新型“液态分离池”Obelisc R色谱柱分离,1%甲酸水溶液与1%甲酸乙腈溶液作为流动相梯度洗脱,四极杆/静电场轨道阱高分辨质谱准确定性并定量。8种待测组分均获得足够的色谱保留和分离,在各自浓度范围内呈现良好的线性关系,相关系数(R^(2))均大于0.99,定量限在0.5~20μg/kg之间,平均回收率在68.0%~104.6%之间,批内与批间RSD均不高于11.3%。该法区别于传统方法:不添加离子对试剂,不使用含缓冲盐流动相,最大限度减少了对质谱检测器的污染;采用高分辨质谱检测器定性定量,结果准确可靠;灵敏度较现行国标显著提高。该方法具有良好的可操作性和重现性,适用于牛奶中氨基糖苷类药物的快速筛查、定性筛选和定量测定。

A method was established for the determination of eight aminoglycoside residues in milk by liquid chromatography quadrupole-orbitrap high resolution mass spectrometry. The samples were exacted and cleaned up by SupelMIP aminoglycosides SPE cartridges prior to analysis by LC-HRMS. The separtion was performed on an Obelisc R column which using liquid separation cell technology by the gradient elution programme using water(1% formic acid) and acetonitrile(1% formic acid). The matrix-matched calibration curve showed good linear with the correlation coefficient R^(2) over 0.99. The limit of quantification was between 0.5 μg/kg and 20 μg/kg. The average recoveris of aminoglycosides ranged from 68.0% to 104.6%, and the relative standard derivations were no more than 11.3%. Compared with traditional technique, this method could reduce contamination to MS detector without using ion-pair regents and buffer solution as mobile phase. Moreover, high resolution mass spectrometry could provide higher accuracy of qualitative and quantitative analysis. The method was operational and reproducible for the analysis of aminoglycoside residues in milk.