超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法测定猪肉中9种大环内酯类抗生素

摘要/Abstract

摘要： 建立了基于超高效液相色谱-四级杆/静电场轨道阱高分辨质谱筛查和确证猪肉中9种大环内酯类抗生素的方法。猪肉样品经乙腈提取，正己烷除脂，用Waters Acquity BEH C18柱（2.1 mm×100 mm，1.7 μm）分离，以甲醇和0.1%甲酸水溶液进行梯度洗脱，在全扫描（full MS）-数据依赖扫描（ddMS2）模式下进行检测。结果表明：9种大环内酯类抗生素的精确质量相对偏差小于1.0×10-6，在0.5～100 ng/mL范围内线性关系良好，相关系数均大于0.998；检出限范围为0.05～0.2 μg/kg，定量限范围为0.1～0.4 μg/kg；加标水平水平为0.1 μg/kg-4.0 μg/kg时，方法回收率为69.4%～107.6%，相对标准偏差低于10%。该方法简便、快速、准确，适用于猪肉中9种大环内酯类抗生素的快速筛查和定量分析。

关键词: 超高效液相色谱, 四级杆/静电场轨道阱高分辨质谱, 猪肉, 大环内酯类抗生素, 检测

Abstract: A rapid method was presented for the determination of 9 macrolides antibiotics in pork sample by ultra-performance liquid chromatography-quadrupole orbitrap high resolution mass spectrometry. Pork samples were extracted by acetonitrile and cleaned with n-hexane, then separated by Waters Acquity BEH C18 column(100 mm×2.1 mm, 1.7 μm) using a binary solvent system composed of methanol and water(0.1% formic acid) by gradient elution. The analytes were determined by quadrupole-orbitrap high resolution mass spectrometry in full-MS and data-dependent scan (ddMS2) mode. The results showed that mass accuracy error of the 9 antibiotics were lower than 1.0×10-6,linear relationships is well in the range of 0.5-100 ng/mL for 9 antibiotics, and correlation coefficients were higher than 0.998. The LOD is in the range of 0.05-0.2 μg/kg and the LOQ is in the range of 0.1-0.4 μg/kg. Recovery of the method is in range of 69.4%-107.6% with spike levels of 0.1-4.0μg/kg, relative standard deviations were lower than 10%. The method is simple, rapid, accurate, which is suitable for the rapid screening and quantitative analysis of 9 kinds of macrolides antibiotics in pork sample.

Key words: ultra high performance liquid chromatography, quadrupole/orbitrap high resolution mass spectrometry, pork samples, macrolides antibiotics, Determination

中图分类号:

O657.63

马俊美孙磊曹梅荣刘茁李强范素芳. 超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法测定猪肉中9种大环内酯类抗生素[J]. 食品科学, 0, (): 0-0.

Zhuo LIU. Determination of 9 kinds of Macrolides Antibiotics in Pork Samples by Ultra Performance Liquid Chromatography-Quadrupole Obitrap High Resolution Mass Spectrometry[J]. FOOD SCIENCE, 0, (): 0-0.

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