气相色谱-质谱检测方法快速筛查保健食品及中成药中8种非甾体抗炎药

GC-MS rapid screening of eight non-steroidal anti-inflammatory drugs in health foods and traditional Chinese medicines

目的:建立保健食品及中成药中非法添加8种非甾体抗炎药物的检测方法。方法:采用溶剂超声或液-液萃取方式对样品进行提取富集,气相色谱-质谱联用(GC-MS),Scan模式进行定性检测,选择离子扫描模式(SIM)进行定量。采用DB-5 ms毛细管色谱柱(30 m×0.25 mm×0.25μm),程序升温:初始温度120℃(1 min),10℃.min-1升至230℃,15℃.min-1升至270℃(20 min),选择EI离子源,溶剂延迟2.5 min,质谱扫描40～350 amu。结果:在选定的色谱条件下,在30 min内快速检测8种非甾体抗炎药物,得到较好的分离;样品筛查结果发现2批样品中分别添加了对乙酰氨基酚和双氯芬酸钠。结论:该法快速﹑准确,专属性强,可用于保健食品及中成药中添加非甾体抗炎药的快速检测。

Objective ： To establish a GC - MS method for detection of non - steroidal anti - inflammatory drugs that illegally added in health foods and traditional Chinese medicines. Method：Samples were extracted and enriched by using solvent extraction or liquid - liquid extraction method. Qualitative detection was carried out by GC - MS and Scan mode. In addition, quantitative analysis was performed using Selected ion monitoring （SIM） mode. The analytical capillary column was DP -5 ms （30 m x0.25 mm x0. 25μm）. The oven temperature was set at 120 ℃ （ 1 min） initially,it was programmed to rise to 230 ℃ at 10 rain ,and then rise to 270 ℃ at 15 ℃ rain-1 20 min）. The FI ion source was selected and the solvent was delayed by 2.5 min. The MS scanning was set at the range of 40 - 350 ainu. Result ： Under the selected chromatographic conditions, 8 kinds of chemical drugs could get a better separation within 30 min. 4 - acetamidophenol and diclofenac sodium were detected in two batches of samples. Conclusion：This method is rapid, accurate, and selective, which is suitable for fast qualitative detection of drugs added illegally.