固相萃取-超高效液相色谱-串联质谱法同时测定保健食品中21种非法添加化合物

建立了固相萃取-超高效液相色谱-串联质谱同时测定保健食品中21种非法添加化合物的方法。样品用乙腈超声提取后,采用HLB固相萃取小柱净化,经Waters BEH C18色谱柱(100 mm×2.1 mm, 1.7 μm)分离,以10 mmol/L 乙酸铵和甲醇为流动相进行梯度洗脱,采用电喷雾电离(ESI)源,在多反应监测模式下检测。结果表明,21种非法添加化合物均呈良好的线性关系,相关系数均≥0.995,不同基质的检出限为3~160 μg/kg ,回收率为61.8%~109.3%,相对标准偏差为1.6%~14.7%。该方法可用于减肥类、降脂类、降糖类、降压类保健食品中21种非法添加药物的同时测定。

Simultaneous determination of 21 illegally added compounds in health foods by ultra high performance liquid chromatography-tandem mass spectrometry with solid phase extraction

A rapid method for the simultaneous determination of 21 illegally added compounds in health foods was developed based on solid phase extraction (SPE) combined with ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). After ultrasonic extraction with acetonitrile, the samples were purified on an HLB SPE column, separated on a Waters BEH C18 column (100 mm×2.1 mm, 1.7 μm) using 10 mmol/L ammonium acetate aqueous solution and methanol as the mobile phases. The compounds were detected by an electrospray ionization (ESI) source in positive ion mode with multi-reaction monitoring (MRM). The 21 illegal additives showed good linear relationships with correlation coefficients no less than 0.995. The limits of detection (LODs) were 3-160 μg/kg for different matrixes. The recoveries ranged from 61.8% to 109.3%, and the relative standard deviations ranged from 1.6% to 14.7%. The method can be used for the simultaneous determination of the illegally added drugs in the losing weight, lipid-lowering, anti-diabetic and anti-hypertension health foods.