Xu Dunming, Lai Guoyin, Chen Yan, Luo Chao, Yi Xionghai, Deng Xiaojun, Feng Feng, Zhang Feng
Technical Center of Xiamen Customs, Xiamen 361026, China.
Technical Center for Animal Plant and Food Inspection and Quarantine, Shanghai Customs, Shanghai 200135, China.
Se Pu. 2019 Jul 8;37(7):778-785. doi: 10.3724/SP.J.1123.2019.01016.
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.
建立了一种基于固相萃取（SPE）结合超高效液相色谱-串联质谱（UHPLC-MS/MS）同时测定保健食品中21种非法添加化合物的快速方法。样品经乙腈超声提取后，在HLB固相萃取柱上净化，采用10 mmol/L乙酸铵水溶液和甲醇作为流动相，在Waters BEH C18柱（100 mm×2.1 mm，1.7 μm）上进行分离。采用电喷雾电离（ESI）源，在正离子模式下进行多反应监测（MRM）检测这些化合物。21种非法添加剂显示出良好的线性关系，相关系数不低于0.995。不同基质的检测限（LOD）为3-160 μg/kg。回收率在61.8%至109.3%之间，相对标准偏差在1.6%至14.7%之间。该方法可用于同时测定减肥、降脂、抗糖尿病和抗高血压保健食品中非法添加的药物。
