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

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×0.25 μm),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×0.25 mm×0.25 μm).The oven temperature was set at 120 ℃ (1 min) initially,it was programmed to rise to 230 ℃ at 10 ℃·min^-1,and then rise to 270 ℃ at 15 ℃·min^-1 20 min).The EI ion source was selected and the solvent was delayed by 2.5 min.The MS scanning was set at the range of 40-350 amu.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.