超高效液相色谱-三重四极杆质谱法测定食品中34种非法添加减肥类化合物

建立了超高效液相色谱-三重四极杆质谱测定食品(含保健食品)中34种减肥类非法添加化合物的方法。采用Waters CORTECS T3色谱柱(100 mm×2.1 mm,2.7μm),以0.1%(v/v)甲酸水溶液-含0.1%(v/v)甲酸的乙腈溶液为流动相,梯度洗脱,在电喷雾离子源、正离子或负离子模式下以多反应监测(MRM)方式检测。西布曲明等29种化合物在0.5~10μg/L范围内、氯噻嗪等5种化合物在2.5~50μg/L范围内均呈良好的线性关系,相关系数(r)均大于0.99;西布曲明等29种化合物在5、10和20μg/kg添加水平下的平均加标回收率为49.2%~136.2%,相对标准偏差(RSD)为0.7%~15.0%(n=6),氯噻嗪等5种化合物在25、50和100μg/kg添加水平下的平均加标回收率为51.5%~130.9%,RSD为0.8%~14.0%(n=6);西布曲明等29种化合物的检出限为5μg/kg,定量限为10μg/kg,氯噻嗪等5种化合物的检出限为25μg/kg,定量限为50μg/kg。本方法已应用于实际样品的测定,共检出了12种化合物,有效打击了非法添加行为。

Determination of 34 illegally adulterated weight loss compounds in foods by ultra high performance liquid chromatography- triple quadrupole mass spectrometry

An analytical method was developed for the determination of 34 illegally adulterated weight loss compounds in foods and dietary supplements by ultra high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-MS/MS). A Waters CORTECS T3 column (100 mm×2.1 mm, 2.7 μm) was used with 0.1% (v/v) formic acid aqueous solution-acetonitrile containing 0.1% (v/v) formic acid as mobile phases by gradient elution. The compounds were detected by electrospray ion source in positive or negative mode with multiple reaction monitoring (MRM) mode. The calibration curves showed good linearity in the range of 0.5-10 μg/L for 29 compounds such as sibutramine, and in the range of 2.5-50 μg/L for five compounds such as chlorothiazide. The correlation coefficients (r) of the standard calibration curves for the 34 analytes were all greater than 0.99. The recoveries of the 29 compounds at spiked levels of 5, 10 and 20 μg/kg were in the range of 49.2%-136.2%, and the RSDs were 0.7%-15.0% (n=6). The recoveries of the five compounds at spiked levels of 25, 50 and 100 μg/kg were in the range of 51.5%-130.9%, and the RSDs were 0.8%-14.0% (n=6). The limits of detection (LODs) and limits of quantification (LOQs) were 5 μg/kg and 10 μg/kg for the 29 compounds, 25 μg/kg and 50 μg/kg for the five compounds, respectively. The method was successfully applied to the analysis of actual samples, and 12 compounds were checked out, which combated the illegal adulteration behavior effectively.