超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速筛查及定量分析保健品中29种非法添加物

Rapid screening and quantitative analysis of 29 kinds of illegally added compounds in diet health foods by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

中文关键词:  四极杆/静电场轨道阱高分辨质谱  快速筛查  非法添加物  保健品

英文关键词:quadrupole/electrostatic field orbitrap high resolution mass spectrometry  rapid screening  illegally added compounds  diet health foods

中文摘要:

      目的 建立超高效液相色谱-四极杆/静电场轨道阱质谱法(ultra performance liquid chromatography- quadrupole/electrostatic field orbitrap high resolution mass spectrometry, UPLC-Q-Orbitrap HRMS)快速筛查及定量分析保健品中常见29种非法添加物的方法。方法 样品用甲醇进行超声提取, 经去离子水稀释后用UPLC-Q-Orbitrap HRMS进行测定。色谱柱选用HSS T3(1.8 μm)柱, 质谱采用全扫描/数据依赖二级扫描模式, 通过一级质谱和二级质谱信息建立的数据库进行高通量筛查及定量分析。对建立的方法进行方法学考察, 并对市售保健品样品进行筛查测定。结果 各组分在0.1~500 ng/mL浓度范围内具有良好的线性, 各化合物的检出限为0.3~20 ng/g, 回收率为68.2%~105.3%, 相对标准偏差为0.4%~11.3%, 能够满足日常检测的要求。结论 该方法简单快捷, 准确度高, 可用于检测保健品中非法添加物的日常监管工作。

英文摘要:

      Objective To establish a method for rapid screening and quantitative analysis of 29 kinds of illegally added compounds in diet health foods by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS). Methods HSS T3 (1.8 μm) column was selected for the chromatographic column, and full scan/data-dependent second-order scanning mode was adopted for the mass spectrometry, and high-throughput screening and quantitative analysis were performed using a database of primary and secondary mass spectra information. The methodology of the established method was investigated, and the samples of health care products were screened and determined. Results Each component had a good linearity in the concentration range of 0.1-500 ng/mL. The detection limits of each compound were 0.3-20 ng/g, and the recoveries were 68.2%-105.3%. The relative standard deviations were 0.4% to 11.3%, which could meet the requirements of daily detection. Conclusion This method is simple, rapid and accurate, which can be used to detect the illegal additives in health products.