超高效液相色谱法同时测定减肥类保健食品中非法添加的25种药物

Simultaneous determination of 25 illegally added drugs in diet health foods by ultra-high performance liquid chromatography

建立了采用超高效液相色谱同时测定减肥类保健食品中25种非法添加化学药物含量的方法.保健食品样品以甲醇为提取溶剂进行超声提取,离心后取上清液以Waters HSS T3色谱柱（100 mm×2.1 mm,1.8 μm）进行分离,乙腈和10 mmol/L乙酸铵水溶液（含0.1％甲酸）为流动相梯度洗脱,流速为0.3 mL/min,在200 ～ 400 nm波长范围内进行定性和定量分析.在相应的浓度范围内,25种化学药物的质量浓度与峰面积呈良好的线性关系,R2≥0.997;定量限在0.500～5.00 ng之间;在低、中、高3个添加水平范围内的平均回收率为70.7％～ 104％,相对标准偏差（RSD）在0.132％ ～ 5.03％之间.样品筛查结果发现,17种减肥保健食品中3种样品非法添加了酚酞,1种样品添加了大黄素.该方法选择性强、分析速度快、高通量,可用于该类保健食品中非法添加化学药品的定性筛查和定量检测.

An analytical method using ultra-high performance liquid chromatography （UPLC） was developed for qualitative and quantitative analysis of 25 illegally added drugs in diet health foods. The diet food samples were extracted using 40 mL methanol by sonication. After centrifu- gation, the supernatants were separated on a Waters HSS T3 column with gradient elution at a flow rate of 0.3 mL/min, coupling with diode array detection （ DAD ） in wavelength range from 200 nm to 400 nm. The binary mobile phase was acetonitrile and l0 mmol/L ammonium acetate solution （ containing 0. 1% formic acid）. The correlation coefficient of standard c：urve for each drug in linearity range was not less than 0. 997, as well as the recoveries of all the drugs in diet health foods were 70. 7%-104% with the relative standard deviations （RSDs） of 0. 132%-5.03% at three spiked levels. Seventeen diet food samples were tested, in which phenolphthalein was found in three samples and emodin was found in one sample. The method is specific, easy, quick, and suitable for confirmation of the 25 illegally added drugs in diet health foods.