超高效液相色谱-串联质谱法测定减肥类保健食品中3种违法添加的缓泻药成分的含量

Determination for 3 kinds of illegally added laxatives in slimming health foods by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  减肥类  保健食品  缓泻药

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  slimming  health food  laxative

中文摘要:

      目的 建立超高效液相色谱-串联质谱法测定减肥类保健食品中脱乙酰比沙可啶、双醋酚丁和比沙可啶3种违法添加的缓泻药含量的方法。方法 样品用甲醇超声提取后, 十八烷基硅烷键合硅胶色谱柱分离, 乙腈-0.1%甲酸水作为流动相洗脱, 以电喷雾离子源正离子模式电离, 结合多反应监测模式采集多个离子对进行测定。结果 3种缓泻药成分在1.0~100 μg/L范围内线性关系良好, 相关系数均大于0.9991, 平均回收率为82.8%~94.6%, 相对标准偏差为4.52%~6.33%, 方法检出限均为25 μg/kg, 定量限均为80 μg/kg。结论 该方法回收率高, 灵敏度高, 重现性好, 操作简便, 适用于实验室的批量测定。

英文摘要:

      Objective To establish a method for determination of 3 kinds of illegal laxatives of deacetyl bisacridine, bisacetophenol and bisacridine in slimming health foods by ultra performance liquid chromatography- tandem mass spectrometry (UPLC-MS). Methods After ultrasonic extraction with methanol, the samples were separated by octyl silane bonded silica gel chromatographic column, and acetonitrile-0.1% formic acid water was eluted as mobile phase. The samples were ionized by electrospray ion source positive ion mode, and multiple ion pairs were collected in combination with multi-reaction monitoring mode for determination. Results The linear relationship of the 3 cathartic ingredients was good in the range of 1.0~100 μg/L, the correlation coefficient was all more than 0.9991, the average recoveries were 82.8%-94.6%, and the relative standard deviations were 4.52%-6.33%, the limit of detection was 25 μg/kg, the limit of quantitative was 80 μg/kg. Conclusion This method has high recovery rate, high sensitivity, good reproducibility, and simple operation. It is suitable for batch determination in the laboratory.