摘要
目的建立高效液相色谱质谱联用技术（HPLC／ESI—MS）的测定方法，测定保健食品中双去甲基西布曲明。方法色谱条件为Johnson SpherigelC18色谱柱（4．6mm×250mm，5μm）；流动相：流动相A液（0．25％乙酸＋20mmol／L乙酸铵），流动相B液（甲醇）=25＋75（体积比），流速1mL／min，检测波长223nm。质谱采用电喷雾正离子模式（ESI＋），分子离子峰m／z252。结果双去甲基西布曲明在0．01～1．20mg／ml范围内，浓度与峰面积呈良好的线性关系，最低检出限为0．95μg／ml（S／N=3）。结论本方法流动相简单，分析时间短且试样预处理简单，灵敏度高，借助质谱的定性能力，可大大提高方法可靠性和抗干扰能力，能准确快速地测定保健食品中的双去甲基西布曲明。
Objective A high-performance liquid chromatography electrospray/mass spectrometry （HPLC/ESI-MS） method was developed to detect N-di-desmethylsibutramine in slimming health food products. Method The separation was completed on a RP-C18 column （4.6 mm × 250 mm, 5 μm） with 0.25% acetic acid aqueous solution containing 20 mmmol/L ammonium acetate as mobile phase. Elution run at a flow rate of 1 ml/min and UV detection was performed at 223 nm. Results Good linearity was shown between the peak area and the concentration of N-di-desmethylsibutramine standards, in a range of 0. 01-1.20 mg/ml. Conclusion The correlation coefficient of the calibration curves was better than O. 9997 （ n = 6）. The limit of detection （LOD） was 0.95 μg/ml （ S/N= 3 ）. The method was sensitive, precise and highly reproducible.
出处
《中国食品卫生杂志》
北大核心
2010年第1期24-26,共3页
Chinese Journal of Food Hygiene
基金
广东医学院青年基金资助项目(xq06027)
关键词
液相色谱-电喷雾质谱联用
双去甲基西布曲明
保健食品
减肥药
High-Performance Liquid Chromatography Electrospray/Mass Spectrometry
N-di-Desmethylsibutramine
Health Food
Anti-Obesity Agents
