HPLC法快速测定保健食品中化学药物添加的研究

Rapid Determination of Chemical Drugs Addition in Health Food by HPLC

采用酸化甲醇超声萃取减肥保健食品中12种可能非法添加的化学药物,固相萃取柱Oasis MCX净化,经二极管阵列检测器测定,利用高效液相色谱法(high performance liquid chromatography,HPLC)测定减肥保健食品中12种非法添加化学药物的含量,并采用液相色谱-串联质谱法对阳性样品进行确证。结果显示:在1.0μg/mL^50.0μg/mL范围内,12种可能非法添加化学药物质量浓度与其色谱峰面积呈良好的线性关系,线性相关系数均大于0.999 5;方法定量限在0.25 mg/kg^1.0 mg/kg,方法检出限在0.08 mg/kg^0.30 mg/kg;回收率在88.6%~102.6%,相对标准偏差在1.2%~3.6%。

High performance liquid chromatography(HPLC)was established to determine the content of 12 kinds of illegally adulterated chemical drugs in weight controlling health foods,which were ultrasonic extracted by acidified methanol,purified by the solid phase extraction column of Oasis MCX,and determined by diode array detector.The positive samples of 12 kinds of illegally adulterated chemical drugs were confirmed by liquid chromatography-mass spectrometry.The results showed that there was a good linear relationship between the mass concentration of 12 possible illegally added chemical drugs and their chromatographic peak area in the range from 1.0μg/mL to 50.0μg/mL,and the correlation coefficient were greater than 0.9995.The limits of quantitation were ranged from 0.25 mg/kg to 1.0 mg/kg,and the limits of detection were ranged from 0.08 mg/kg to 0.30 mg/kg.The average recoveries were ranged from 88.6%to 102.6%,and the relative standard deviations ranged from 1.2%to 3.6%.