Objective]To establish a rapid resolution liquid chromatography-mass spectrometry(RRLC-MS) method for sibutramine hydrochloride, ephedrine hydrochloride and furosemide, which is the illegally added substances in diet pills. [Method]The chromatographic conditions: Agilent SB-C18 column(2.1mm×50mm, 5μm). The mobile phase consists of acetonitrile(containing 0.1% formic acid) and 0.1% formic acid solution, gradient elution with flow rate of 0.2mL·min-1; The MS conditions: electrospray ionization(ESI) source, with positive and negative ions, multiple reaction monitoring(MRM) mode to detect contents of prohibited substances in diet pills. [Result]Under the above conditions, all seven diet pills were detected with the sibutramine hydrochloride and ephedrine hydrochloride. The concentration range of the two substances was from 0.39 to 4.29μg·g-1 and from 1.63 to 8984.18μg·g-1 respectively. One drug contained furosemide, while the content was 8.71μg·g-1. [Conclusion]The method established was fast, convenient, had high sensitivity and high accuracy, which can detect prohibited substances quantitatively and qualitatively in diet pills.%[目的]建立盐酸西布曲明、呋塞米和盐酸麻黄碱的快速高分离液相色谱-质谱联用（rapid resolution liquid chromatography-mass spectrometry, RRLC-MS）方法，检测7种减肥药中是否含有非法添加成分。[方法]色谱条件：Agilent SB-C18柱（2.1mm×50mm,5μm），乙腈（含0.1%甲酸）-0.1%甲酸水溶液为流动相进行梯度洗脱，流速0.2mL·min-1；质谱条件：电喷雾离子（electrospray ionization, ESI）源，以正负离子、多反应监测（multiple reaction monitoring, MRM）扫描模式检测减肥药中违禁成分。[结果]7种减肥药中均检测到盐酸西布曲明和盐酸麻黄碱，含量范围分别为0.39～4.29μg·g-1和1.63～8984.18μg·g-1，1种减肥药中检测到呋塞米，含量为8.71μg·g-1。[结论]本研究建立的快速高分离液相色谱-质谱联用法方便快捷、灵敏度好、准确度高，适用于减肥药中非法添加成分的定性定量检测。
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