目的建立了液相色谱-离子阱质谱联用定性测定48种磺胺类、喹诺酮类,四环素类、氯霉素类、大环内酯类和抗真菌类的方法,并用于中成药和保健食品非法添加的检测。方法样品通过甲醇超声振荡提取,其液相色谱分离采用Agilent Eclipse Plus C18柱,流动相A为0.2%甲酸,流动相B为甲醇,梯度洗脱;使用Ion-trap LC/MS分析模式,电喷雾离子源、正离子模式检测。通过与标准谱库中保留时间和多级质谱图的数据进行比对,定性确定样品中添加的抗生素种类。结果 10批中成药中有1批检出氧氟沙星,25批保健食品中有7批检出磺胺甲噁唑。结论本方法解决了5对同分异构体的分离和质谱鉴定问题,并实现同一液质系统内分析多种结构类型的化合物,特别适合中成药和保健食品中违禁抗生素类化学药品的测定。
AIM To use Ion-trap LC / MS to qualitatively analyze forty-eight antibiotics including sulfanilamides,quinolones,tetracyclines,chloram phenicols,macrolides and antifungal agents.The method has been applied to the illegal acts in traditional Chinese patent medicines and health foods.METHODS The test solutions of samples were prepared by combining ultrasonic extraction and disintegration.Separation was performed on an Agilent Eclipse Plus C18 column with the binary mobile phase consisting of 0.2% formic acid( solvent A) and methanol( solvent B) in a gradient elution mode,Ion-trap LC / MS analytic pattern and the electrospray ionization source in positive ion mode.Comparing with retention time and spectrums of references in library set up,the target compounds in sample were screened and identified.RESULTS Ofloxacin was found in one out of ten samples and sulfamethoxazole was found in seven samples out of twenty-five batches of health foods.CONCLUSION The method has solved the problem of separation of five pairs of isomers and qualitative analysis by MS.Several structure kinds of compounds can be analyzed in one system.It is quite suitable for confirmation of illegally added antibiotics drugs in medicines and health foods.