色谱

色谱 ›› 2019, Vol. 37 ›› Issue (9): 1011-1018.DOI: 10.3724/SP.J.1123.2019.01044

• 技术与应用 • 上一篇    下一篇

超高效液相色谱-四极杆静电场轨道离子阱质谱同时检测动物源性食品中20种β-受体阻滞剂及代谢物

聂雪梅1, 董旭阳1,2, 许秀丽1, 张峰1   

  1. 1. 中国检验检疫科学研究院, 北京, 100176;
    2. 陕西科技大学, 西安, 710021
  • 收稿日期:2019-01-25 出版日期:2019-09-08 发布日期:2015-07-30
  • 通讯作者: 张峰
  • 基金资助:
    国家重点研发计划（2016YFF0203903）.

Determination of 20 β -blockers and metabolites in animal-origin foods by ultra performance liquid chromatography-quadrupole electrostatic field orbitrap mass spectrometry

NIE Xuemei1, DONG Xuyang1,2, XU Xiuli1, ZHANG Feng1   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100176, China;
    2. Shanxi University of Science and Technology, Xi'an 710021, China
  • Received:2019-01-25 Online:2019-09-08 Published:2015-07-30
  • Supported by:
    National Key R&D Program of China (No. 2016YFF0203903).

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摘要： 采用超高效液相色谱-四极杆静电场轨道离子阱质谱法，建立了动物源性食品中20种β-受体阻滞剂及其代谢物的高通量筛查分析方法。通过对前处理条件和仪器条件的优化，提高了灵敏度和适用性。最终选用低温高速离心的方式净化样品，C8色谱柱分离待测化合物，在数据依赖性质谱扫描模式下对目标物进行定性、定量分析。20种目标物在0.1~10 μg/L线性范围内呈良好的线性关系，相关系数（r2）均大于0.99。该方法的检出限为1~5 μg/kg，定量限为2~10 μg/kg，平均回收率在60.37%~100.84%，相对标准偏差均小于10%。该法操作简单，重现性好，准确度高，适用于动物源性食品中的β-阻滞剂及其代谢产物残留的筛查分析。

关键词: -受体阻滞剂及代谢物, &beta, 超高效液相色谱, 动物源性食品, 高分辨质谱, 高通量筛查

Abstract: In this study, ultra performance liquid chromatography-quadrupole electrostatic field orbitrap mass spectrometry was used to establish a high-throughput screening method for 20 β -blockers and their metabolites in foods of animal origin. The sensitivity and applicability of the established method were improved by optimizing the instrument and pretreatment conditions. The samples were purified by high speed centrifugation at low temperature, and the compounds were separated by a C8 column. Qualitative and quantitative analyses of the compounds were performed in full MS/dd-MS2 (data-dependent MS2) mode. Twenty compounds showed a good linear relationship in the range 0.1-10 μg/L, with correlation coefficients (r2) greater than 0.99. The limits of detection (LODs) ranged from 1 to 5 μg/kg, while the limits of quantification (LOQs) ranged from 2 to 10 μg/kg. The average recoveries were 60.37%-100.84%, with relative standard deviations less than 10%. The method is operationally simple and has good reproducibility and high accuracy, which are essential for β -blockers and metabolite residue screening in foods of animal-origin.

Key words: β -blockers and metabolite, foods of animal origin, high-resolution mass spectrometry, high-throughput screening, ultra performance liquid chromatography (UHPLC)

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