In this paper, an ultra-high-performance liquid chromatography coupled with linear ion trap quadrupole Orbitrap high resolution mass spectrometry (UHPLC-LTQ-Orbitrap HRMS) method was developed and validated for identification, confirmation and quantitation of illegal adulterated weight-loss drugs in plant dietary supplements. 13 wt-loss drugs were well separated by the gradient elution of 10 mmol/L ammonium acetate − 0.05% formic acid H₂O and acetonitrile at a flow rate of 0.2 mL/min within 12 min. The MS analysis was operated under the positive ion and in full MS/dd-MS² (data-dependent MS²) mode. The full MS scan with resolution at 60 000 FWHM and narrow mass windows at 5 ppm acquired data for identification and quantitation, and dd-MS² scan with resolution at 15 000 FWHM obtained product ions for confirmation. The method validation showed good linearity with coefficients of determination (r²) higher than 0.9951 for all analytes. Meantime, all the LOD and LLOQ values were in the respective range of 0.3–2 and 1–9 ng/g. The accuracy, intra- and inter-day precision were in the ranges of −1.7 to 3.4%, 1.7–5.0% and 1.9–4.4%, respectively. The mean recoveries ranged from 85.4 to 107.1%, while the absolute and relative matrix effect were in the corresponding range of 98.2–108.6% and 2.6–8.7%. Among 120 batches of weight loss plant dietary supplements, sibutramine and fluoxertine or both were positive in 29 samples. In general, LTQ-Orbitrap HRMS technology was a powerful tool for the analysis of illegal ingredients in dietary supplements.

本文开发了一种超高效液相色谱-线性离子阱四极杆Orbitrap高分辨率质谱（UHPLC-LTQ-Orbitrap HRMS）方法，并已用于鉴定，确认和定量非法掺假减肥药。植物膳食补充剂。通过在12分钟内以0.2 mL / min的流速梯度洗脱10 mmol / L醋酸铵-0.05％甲酸H ₂ O和乙腈，可以很好地分离出13种失重药物。MS分析在阳离子下并在完全MS / dd-MS ²（数据相关的MS ²）模式下进行。完整的MS扫描，分辨率为60000 FWHM，窄质量窗口为5 ppm，用于鉴定和定量数据，以及dd-MS ²以15 000 FWHM的分辨率扫描得到的产物离子以进行确认。方法验证显示出良好的线性，所有分析物的测定系数（r ²）均高于0.9951。同时，所有LOD和LLOQ值分别在0.3–2和1–9 ng / g的范围内。精度，日内和日间精度分别在-1.7至3.4％，1.7-5.0％和1.9-4.4％的范围内。平均回收率在85.4％至107.1％之间，而绝对和相对基质效应分别在98.2–108.6％和2.6–8.7％的范围内。在120批次的减肥植物膳食补充剂中，29份样品中的西布曲明和氟西汀或两者均为阳性。通常，LTQ-Orbitrap HRMS技术是分析膳食补充剂中非法成分的强大工具。