摘要
提出了减肥保健食品中违禁添加药物利莫那班的高效液相色谱-串联质谱分析方法。不同类型的减肥保健食品经加速溶剂萃取及固相萃取净化后,以Waters Atlantis T_3分离柱,以甲醇-10 mmol·L^(-1)乙酸铵混合溶液为流动相,采用多反应监测正离子模式检测,定性离子对为m/z462.9,363.0,m/z 462.9,84.0,定量离子对为m/z 462.9,363.0。线性范围为0.2～500μg·L^(-1),检出限(3S/N)为0.75 mg·kg^(-1)。加标回收率为83.7%～101.6%,日内和日间精密度(n=6)分别小于8%和10%。
HPLC-MS/MS was applied to the determination of rimonabant, a contraband drug added in some de-obese health-care foodstuffs. Rimonabant in different kinds of such foodstuffs were separated from the sample and purified by accelerated solvent extraction and solid phase extraction in succession. The eluate was used for HPLC-MS/MS determination, in which the Waters Atlantis T3 column was used as chromatographic column, and a mixture of methanol and 10 mmol · L^-1 ammonium acetate solution was used as mobile phase; positive electrospray ionization as well as multiple reaction monitoring mode was used in the detection. Ion pairs used for qualitative analysis were： m/z 462. 9, 363. 0 and m/z 462. 9, 84. 0, ion pair use for quantitative analysis was m/z 462. 9, 363.0. Linearity range was found between 0. 2- 500 μg · L^-1, and the detection limit （3S/N） found was 0. 75 mg · kg^-1. Values of recovery found by addition of standard rimonahant, were in the range of 83. 7%- 101.6%, and values of RSD＇s （n=6） of intra-day and inter-day found were less than 8% and 10% respectively.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2009年第10期1145-1149,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家科技支撑计划农业领域课题(2006BAD27B02)
