建立了分散液液微萃取-反萃取-接受相固化与高效液相色谱联用测定减肥茶中西布曲明的方法。优化的条件为:400"L石油醚为萃取剂、120"L甲醇为分散剂、14"L 0.2 mol/L HCl溶液和1"L甲醇的混合溶液为接受相,萃取2 min。在优化条件下西布曲明的富集因子可达130倍。方法的线性范围为0.6~200"g/L,检测出限为0.2"g/L,定量限为0.6"g/L。样品加标回收率介于91.9%~108.4%,日间相对标准偏差小于14%。
A novel method for the determination of sibutramine in dietic teas by dispersive liquid-liquid microextraction-back extraction-solidification of acceptor phase(DLLME-BE-SAP)-high performance liquid chromatography was developed.The optimal experimental conditions were as follows: 400 μL petroleum ether as the organic phase,120 μL methanol as the dispersive solvent,the mixture of 14 μL of 0.2 mol/L HCl and 1 μL methanol as the acceptor phase.The extraction time was 2 min.High enrichment factor(130-fold) of sibutramine was obtained under the optimal experimental conditions.The linear range was 0.6-200 μg/L.The limit of detection(S/N=3) was 0.2 μg/L and the limit of quantitation(S/N=10) was 0.6 μg/L.The recoveries of the spiked samples were from 91.9% to 108.4%,and the inter-day relative standard deviations were lower than 14.0%.