液相色谱-离子阱质谱法同时测定减肥类保健食品中非法添加的12种化学药物

Simultaneous determination of 12 kinds of chemical drugs illegally mixed into slimming health foods by liquid chromatography-ion trap mass spectrometry

目的建立液相色谱-离子阱质谱法同时测定减肥类保健食品中12种非法添加化学药物的分析方法,并对56批抽检样品进行检测。方法样品经甲醇超声提取后,经SHISEIDOCAPCELL-PAKC18色谱柱(150mm×4.6mm,5μm)分离,以乙酸铵溶液-甲醇为流动相,梯度洗脱。采用电喷雾离子源(electrospray ionization,ESI)的正离子扫描模式对样品中非法添加的12种化合物进行定性检测。结果该法能够同时完成对减肥类保健食品中12种非法添加化学药物的检测,方法检出限为0.1~0.5 ng/mL。采用该法对56批抽检样品进行检验,其中13批检出西布曲明和N-单去甲基西布曲明,4批检出奥利司他,阳性检出率为30%。结论该法专属性好、灵敏度高、简便快速,可用于减肥类保健食品中非法添加化学药物的快速筛查。

Objective To establish an analytical method for the simultaneous determination of 12 kinds of chemical drugs illegally mixed into slimming health foods by liquid chromatography-ion trap mass spectrometry and test 56 batches of sampling samples. Methods After ultrasonic extraction with methanol, the samples were separated on a SHISEIDO CAPCELL-PAK C18 column(150 mm×4.6 mm, 5 μm) with ammonium acetate solution-methanol as the mobile phase and gradient elution. 12 kinds of compounds illegally mixed in the samples were qualitatively detected by electrospray ionization(ESI) in positive ion scanning mode. Results The method could simultaneously detect 12 kinds of chemical drugs illegally mixed into slimming health foods with the detection limits of 0.1-0.5 ng/mL. The method was used for the detection of 56 batches of randomly selected samples, among which sibutramine and N-monodesmethyl sibutramine were detected in 13 batches, and orlistat was detected in 4 batches, with the positive detection rate was 30%. Conclusion This method is specific, sensitive, simple and rapid, and can be used for rapid screening of chemical drugs illegally mixed into slimming health foods.