摘要
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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2012年第10期1847-1852,共6页
Chinese Journal of Pharmaceutical Analysis
基金
陕西省科技厅科技研究发展计划项目(No.2009K13-03)
关键词
气相色谱-质谱
非甾体抗炎药物
布洛芬
对乙酰氨基酚
安替比林
氨基比林
甲芬钠酸
双氯芬酸
尼美舒利
贝诺酯
保健食品
中成药
非法添加监测
gas chromatography - mass spectrometry ( GC - MS )
non - steroidal anti - inflammatory drugs(NSAIDs)
ibuprofen
4 - acetamidophenol
antipyrine
aminophenazone
mefenamic acid
diclofenac
nimesulide
benorilate health foods
traditional Chinese medicines
added illegally monitor