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减肥类保健品中20种非法添加药物

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减肥类保健品中常见20种非法添加药物。方法保健品样品以甲醇为提取溶剂进行超声提取,然后使用UPLC-Q-Orbitrap HRMS进行测定,采用全扫描/数据依赖的二级扫描(Full MS/dd-MS~2)扫描模式。通过比较样品与标准品的色谱保留时间、一级质谱和二级质谱,确定样品中是否掺杂了减肥药物,并对阳性样品进行定量分析。结果建立的Q-Orbitrap方法简便快捷、定性能力强,非常适合高通量非法添加筛查。20种减肥药物在0.1～300 ng/mL范围内具有良好的线性,线性相关系数均大于0.995,各类药物的检出限为0.03～10 ng/mL,回收率为78.5%～98.6%,相对标准偏差为2.11%～9.21%。结论该方法操作简单,分析时间短,灵敏度高,准确可靠,为打击日益猖獗的非法添加行为提供了新的手段。

Rapid screening and quantitative detection of 20 kinds of illegally added drugs in diet health foods by ultra performance liquid chromatography- quadrupole/electrostatic field orbitrap high resolution mass spectrometry

Objective To establish a method for rapid screening and quantitative detection of 20 kinds of illegally added drugs in diet health foods by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS). Methods The diet food samples were extracted using methanol by sonication, and then the supernatants were detected by UPLC-Q-Orbitrap HRMS with Full MS/dd-MS2 mode. By comparing the chromatographic retention time, mass spectrometry and two stage mass spectrometry of samples and standard products, it could be determined that the samples were adulterated with weight-loss drugs or not, and then the positive samples were analyzed. Results The established method possessed powerful qualitative ability and high sensitivity. The results indicated that the linearity of all 20 kinds of drugs ranged from 0.1 to 300 ng/mL with the correlation coefficients more than 0.995. The limits of detection were 0.03~10 ng/mL for the 20 kinds of drugs. The recoveries were 78.5%~98.6%, and the relative standard deviations were 2.11%~9.21%. Conclusion This established method is rapid, accurate and highly selective, which provides a powerful tool for the combating with rampant illegal adulteration behaviors.