减肥保健食品中西布曲明及其活性代谢物总量的测定

Determination of Total Amount of Sibutramine and Its Active Metabolites in Weight-reducing Food

目的:建立液相色谱和液相色谱-质谱法测定减肥保健食品中西布曲明及其活性代谢物总量的检测方法。方法:在冰水浴中,样品与甲基化试剂甲醛和硼氢化钾作用,样品中西布曲明活性代谢物定量转化成西布曲明,以液相色谱和液相色谱-质谱法检测样品中西布曲明的总量。结果:本方法线性范围为10～200mg/L,回归方程为y=89.59847x-1.05361,相关系数r=0.99993,最低检出限为1mg/kg,相对标准偏差为4.5%,回收率为83%。结论:该方法简单、准确、快速,灵敏度高、选择性好,适用于减肥保健食品中西布曲明及其活性代谢物总量的测定。

Objective： To establish a HPLC and HPLC-MS method for determining the total amount of sibutramine and its active metabolites,N-desmethyl sibutramine and N-di-desmethyl sibutramine in weight-reducing food.Methods： Samples were subjected to methylation treatment with formaldehyde and potassium borohydride in ice bath in order to convert active sibutramine metabolites into sibutramine.Results： The linear range of the method was between 10 and 200 mg/L and the regression equation was y = 89.59847x-1.05361 with a correlation coefficient of 0.9999.The detection limit was 1 mg/kg.The average recovery for the total amount of sibutramine and its active metabolites was 83% with a RSD of 4.5%.Conclusion： The established method is simple,accurate and rapid and has good selectivity.It is most suitable for determining total amount of sibutramine and its active metabolites in weight-reducing food.