超高效液相色谱-四极杆-静电场轨道阱高分辨质谱快速筛查与确证猪尿中74种抗生素及其他化合物

采用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UPLC-Q-ExactiveOrbitrap)建立了猪尿中74种抗生素及其他化合物的快速筛查与确证方法。猪尿样品经高速离心并稀释后,以AgilentSBC18色谱柱(3.0mm×100mm,1.8μm)分离,0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相进行梯度洗脱。结合精确分子质量数、保留时间和二级特征碎片离子对目标化合物进行筛查与确证。74种目标药物在各自的浓度范围内呈良好线性(r2>0.99),检出限(LOD)为10ng/mL,在检出限加标浓度下,回收率集中在55.8%~120%,相对标准偏差(RSD)为1.3%~21%。该方法简便、快速、灵敏、准确,适用于猪尿中多种抗生素及其他化合物的定性确证,有利于掌握养殖业用药情况。

Rapid Screening and Confirmation of 74 Antibiotics and Other Compounds in Swine Urine by Ultra Performance Liquid Chromatography-Quadrupole-Exactive Orbitrap Mass Spectrometry

An ultra performance liquid chromatography-quadrupole-exactive orbitrap mass spectrometry (UPLC-Q-Exactive Orbitrap ) was developed for the rapid screening and confirmation of 74 antibiotics and other compounds in swine urine.The samples were high-speedily centrifuged,then diluted with solvent,and finally separated on an Agilent SB C18 (3.0 mm×100 mm,1.8 μm ) column using a binary solvent system composed of 0.1 % formic acid aqueous solution and 0.1 % formic acid acetonitrile solution by gradient elution.Under the optimal conditions,the analytes were precisely screened and confirmed with the precision mass,retention time and two-stage ion mass spectra.There were good linear relationships for 74 analytes in their respective concentration ranges with correlation coefficients ( r2 ) larger than 0.99 and limits of detection (LOD ) of10 ng/mL.The recoveries for 74 compounds in swine urine at LOD spiked level mainly ranged from 55.8 % to120 %,with relative standard deviations (RSD ) of1.3 %-21 %.The method was convenient,rapid,sensitive and accurate,and was quite effective for the screening and confirmation of 74 antibiotics and other compounds in swine urine,which was beneficial to the investigation on drugs situation in husbandry.