Food and Drug Administration, Division of Pharmaceutical Analysis, 1114 Market St., St. Louis, MO 63101, United States.
J Pharm Biomed Anal. 2011 Feb 20;54(3):469-74. doi: 10.1016/j.jpba.2010.09.017. Epub 2010 Sep 19.
In response to recent incidents of undeclared sibutramine, an appetite suppressant found in dietary supplements, we developed a method to detect sibutramine using hand-held ion mobility spectrometers with an analysis time of 15 s. Ion mobility spectrometry is a high-throughput and sensitive technique that has been used for illicit drug, explosive, volatile organic compound and chemical warfare detection. We evaluated a hand-held ion mobility spectrometer as a tool for the analysis of supplement extracts containing sibutramine. The overall instrumental limit of detection of five portable ion mobility spectrometers was 2 ng of sibutramine HCl. When sample extractions containing 30 ng/μl or greater of sibutramine were analyzed, saturation of the ionization chamber of the spectrometer occurred and the instrument required more than three cleaning cycles to remove the drug. Hence, supplement samples suspected of containing sibutramine should be prepared at concentrations of 2-20 ng/μl. To obtain this target concentration range for products containing unknown amounts of sibutramine, we provided a simple sample preparation procedure, allowing the U.S. Food and Drug Administration or other agencies to screen products using the portable ion mobility spectrometer.
针对最近在膳食补充剂中发现未申报的安非他命类食欲抑制剂西布曲明的事件,我们开发了一种使用手持式离子淌度谱仪在 15 秒内检测西布曲明的方法。离子淌度谱仪是一种高通量、高灵敏度的技术,已用于非法药物、爆炸物、挥发性有机化合物和化学战剂的检测。我们评估了手持式离子淌度谱仪作为分析含有西布曲明的补充剂提取物的工具。五台便携式离子淌度谱仪的整体仪器检出限为 2 纳克盐酸西布曲明。当分析含有 30 纳克/微升或更高浓度西布曲明的样品提取液时,谱仪的离子化室会发生饱和,仪器需要超过三个清洗循环才能清除药物。因此,怀疑含有西布曲明的补充剂样品应制备成 2-20 纳克/微升的浓度。为了获得含有未知量西布曲明的产品的这个目标浓度范围,我们提供了一种简单的样品制备程序,使美国食品和药物管理局或其他机构能够使用便携式离子淌度谱仪对产品进行筛选。