食品科学 ›› 2020, Vol. 41 ›› Issue (4): 273-279.doi: 10.7506/spkx1002-6630-20181026-306

• 安全检测 • 上一篇    下一篇

超高效液相色谱-四极杆/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

马俊美,孙磊,曹梅荣,刘茁,李强,范素芳   

  1. (1.河北省食品检验研究院,河北 石家庄 050000;2.河北科技大学生物科学与工程学院,河北 石家庄 050018)
  • 出版日期:2020-02-25 发布日期:2020-03-02
  • 基金资助:
    国家重大科学仪器设备开发专项(2012YQ03011110)

Determination of Nine Macrolide Antibiotics in Pork Samples by Ultra-high Performance Liquid Chromatography Quadrupole/Orbitrap High Resolution Mass Spectrometry

MA Junmei, SUN Lei, CAO Meirong, LIU Zhuo, LI Qiang, FAN Sufang   

  1. (1. Hebei Food Inspection and Research Institute, Shijiazhuang 050000, China; 2. College of Bioscience and Bioengineering, Hebei University of Science and Technology, Shijiazhuang 050018, China)
  • Online:2020-02-25 Published:2020-03-02

摘要: 建立基于超高效液相色谱-四极杆/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%甲酸溶液进行梯度洗脱,在全扫描-数据依赖扫描模式下进行检测。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;加标量为0.1~4.0 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, 四极杆/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 macrolide antibiotics in pork samples by ultra-high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry. The samples were extracted with acetonitrile and the extract was defatted with n-hexane and then separated with a Waters Acquity BEH C18 column (2.1 mm × 100 mm, 1.7 μm) by gradient elution using a binary solvent system composed of methanol and 0.1% formic acid in water. The analytes were detected by quadrupole-orbitrap high resolution mass spectrometry in the full-scan and data-dependent scan (ddMS2) mode. The results showed that the deviation between the theoretical and measured accurate mass-to-charge ratio was lower than 1.0 × 10-6, and good linear relationships were observed in the concentration range of 0.5–100 ng/mL for the 9 antibiotics with correlation coefficients higher than 0.998. The limits of detection were in the range of 0.05–0.2 μg/kg and the limits of quantification were in the range of 0.1–0.4 μg/kg. The recoveries of the method ranged from 69.4% to 107.6% at spiked concentration levels of 0.1–4.0 μg/kg, with relative standard deviations (RSDs) lower than 10%. This method proved to be simple, rapid, and accurate, and therefore it was suitable for rapid screening for and quantitative analysis of 9 macrolides antibiotics in pork samples.

Key words: ultra-high performance liquid chromatography, quadrupole/orbitrap high resolution mass spectrometry, pork samples, macrolide antibiotics, determination

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