高效液相色谱-质谱联用测定减肥保健品中的痕量西布曲明

目的：在已有分析鉴定西布曲明的添加检验方法的基础上,建立了高效液相色谱-质谱联用检测痕量西布曲明的方法.方法：以C18为色谱柱,采用多反应离子监测（MRM）技术,在优化实验条件下,选择280.2/125.1离子对为检测对象,对西布曲明进行鉴别和定量分析.结果：西布曲明在0.17~ 8.34 μg·mL-1范围内与280.2/125.1提取离子流峰面积有良好的线性关系,相关系数r=0.9997,检出限为10 pg,样品的平均加样回收率为99.79%,RSD为0.28%（n=3）.结论：本文建立的方法准确、可靠,较现有方法更加灵敏,可用于西布曲明的添加检验.

Determination of Trace Sibutramine in Weight-loss Healthy Food by HPLC/MS

Objective： Based on the existing detection method of sibutramine, an HPLC/MS method for identification and quantitative analysis of trace sibutramine in weight-loss healthy food had been developed. Method： The separation was conducted by C18 column. In the optimized experimental conditions, the ion pair（280. 2/125.1 ） was selected as the monitoring object. The sibutramine was iden-tified and quantitative analyzed with mass spectrum in the multiple-reaction monitoring （MRM） mode via positive electrospray ioniza-tion. Result： Good liner relationship was achieved when the linear concentration range of sibutramine was 0. 17 - 8. 34 μg · mL^-1 （ r = 0. 9997 ）. The detection limits was 10 pg and the average recovery rate was 99. 79% （RSD = 0. 28% , n = 3 ）. Conclusion： The im-proved method is accurate, reliable, more sensitive than the existing method, and it can be used for quantitative and qualitative tests of sibutramine.