超高效液相色谱-四级杆-静电场轨道肼高分辨质谱筛查测定饲料中19种磺胺类药物

Screening and Confirmation of 19 Sulfonamides in Feed by Ultra High Performance Liquid Chromatography- quadrupole- exactive Orbitrap Mass Spectrometry

建立了超高效液相色谱-四级杆-静电场轨道阱高分辨质谱联用（UPLC-Q-Exactive Orbitrap）快速筛查和确证定量饲料中19种磺胺类药物的分析方法。饲料样品经乙腈-0.1%甲酸溶液（80：20,V/V）超声提取,Agilent SB C18色谱柱（100 mm×3.0 mm,1.8μm）分离,以0.1%（V/V）甲酸乙腈溶液和0.1%（V/V）甲酸水溶液为流动相进行梯度洗脱。静电场轨道阱全扫描得到磺胺类药物的一级精确质量数与理论精确相对分子质量对比,相对质量偏差在0.006×10-6-1.252×10-6之间,有效去除了基质干扰,实现对饲料中磺胺类药物的快速筛查;同时建立了19种磺胺类药物的二级质谱数据库,实现对19种磺胺类药物的定性筛查及同步定量。19种磺胺类药物在0.1-200μg/L浓度范围内线性关系良好r〉0.99,方法检测限为50μg/kg,回收率在59.61%-106.45%之间。

An ultra high performance liquid chromatography- quadrupole- exactive orbitrap mass spectrometry method（ UPLC- Q- Exactive Orbitrap） was developed for rapid screening,confirmation and quantitative of 19 sulfonamides in feed. The samples were extracted with acetonitrile- 0. 1% aqueous formic acid solution（ 80∶ 20,V / V）,and the extracts were then separated on an Agilent SB C18（ 50 mm × 3. 0 mm,1. 8 μm） using a binary solvent system composed of 0. 1% formic acid acetonitrile solution and 0. 1% aqueous formic acid solution by gradient elution. The relative molecular masses of the target compounds were obtained in full scan mode with a relative deviation in the range of 0. 006 × 10- 6~ 1. 252 × 10- 6compared to the theoretical value,indicating effective elimination of the matrix interference. Tandem mass spectrometric database based on characteristic fragment ions for the 19 sulfonamides was built. This method allowed qualitative screening and quantitative analysis at the same time. Calibration curve was linear between 0. 1 and 200 μg / L,with the correlation coefficient r 0. 99. The limit of detection was 50 μg / kg. The recovery in feed was from 59. 61% to 106. 45%.