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

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

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。

An analytical method was developed for the determination of34illegally adulterated weight loss compounds in foods and dietary supplements by ultra high performance liquid chromatography-triple quadrupole mass spectrometry(UHPLC-M^^MS).A Waters CORTECS T3column(100mmx2.1mm,2.7pm)was used with0.1%(v/v)formic acid aqueous solutionacetonitrile containing0.1%(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 of0.5-10pg/L for29compounds such as sibutramine,and in the range of2.5-50pg/L for five compounds such as chlorothiazide.The correlation coefficients(r)of the standard calibration curves for the34analytes were all greater than0.99.The recoveries of the29compounds at spiked levels of5,10and20pg/kg were in the range of49.2%-136.2%,and the RSDs were0.7%-15.0%(n=6).The recoveries of the five compounds at spiked levels of25,50and100pg/kg were in the range of51.5%-130.9%,and the RSDs were0.8%-14.0%(n=6).The limits of detection(LODs)and limits of quantification(LOQs)were5pg/kg and10pg/kg for the29compounds,25pg/kg and50pg/kg for the five compounds,respectively.The method was successfully applied to the analysis of actual samples,and12compounds were checked out,which combated the illegal adulteration behavior effectively.