抗风湿类中成药和保健食品中非法添加化学成分的高液相色谱-质谱/质谱法检测  

Rapid determination of chemicals added illegally in anti-rheumatic traditional Chinese medicines and health products by HPLC-MS/MS

作　　者：黎雪清[1] 鲁艺[1] 王铁杰[1] 殷果[1] 韩东岐[1] 江坤[1] 

机构地区：[1]广东省深圳市药品检验所 深圳药品质量标准研究重点实验室,广东深圳518057

出　　处：《中国医药导报》2015年第6期86-90,共5页China Medical Herald

基　　金：广东省深圳市基础研究项目(编号JCYJ20120618153944322)

摘　　要：目的建立一种快速检测抗风湿类中成药和保健食品中30种非法添加化学成分的高液相色谱-质谱/质谱法。方法色谱条件：C18（4.6 mm×250 mm,5μm）色谱柱,以甲醇-0.1%乙酸溶液为流动相,梯度洗脱,质谱条件：电喷雾离子化正离子检测（ESI＋）,全扫描一级质谱、选择离子二级扫描质谱检测方式,扫描范围50-800 aum,对抗风湿类中成药和保健食品中非法添加的化学成分进行快速定性分析。结果根据检测到的化合物的色谱保留时间及一级、二级质谱信息,并与对照品比较,可作为分析抗风湿类中成药和保健食品中非法添加吗啡、甲氧苄啶、对乙酰氨基酚、罗通定、氨基比林、龙胆苦苷、磺胺甲恶唑、安替比林、阿司匹林、非那西丁、盐酸美沙酮、泼尼松、可的松、异丙安替比林、吡罗昔康、氢化可的松、金诺芬、地塞米松、甲基泼尼松龙、醋酸曲安奈德、酮洛芬、舒林酸、萘普生、地西泮、醋酸地塞米松、保泰松、奥沙普秦、双氯芬酸钠、吲哚美辛和丙酸倍氯米松等30种化学成分的有效手段。在50批供试品中,检测到有10种供试品中含有非法添加的化学成分。结论本方法专属性强、灵敏度高,可作为抗风湿类中成药和保健食品中非法添加化学成分的快速检测方法。Objective To establish an HPLC-MS/MS method for rapid determination of 30 chemicals added illegally in anti-rheumatic traditional Chinese medicines and health products. Methods The HPLC chromatographic determination was condcted on C18 column（4.6 mm×250 mm, 5 μm）. The gradient elution was done with the mixed solution of methanol-0.1% acetic acid. The mass spectrometer condition was as follows： the ionition mode was ESI＋, the mode was mass scan and daughter scan with scan range from 50 to 800 aum, and the chemicals in sample were rapid screended and identified. Results Chemicals added illegally, ncluding Morphine, Trimethoprim, Paracetamol, Rotundine, Aminopyrine,Gentiopicroside, Sulfamethoxazole, Phenazone, Aspirin, Phenacetin, Methadone hydrochloride, Prednisone, Cortisone,Propyphenazone, Piroxicam, Hydrocortisone, Auranofin, Dexamethasone, Methylprednisolone, Triamcinolone acetonide acetate, Ketoprofen, Sulindac, Naproxen, Diazepam, Dexamethasone acetate, Phenylbutazone, Oxaprozin, Diclofenac sodium, Indomethacin and Beclomethasone dipropionate, were identified according to the spectrum, chromatogramphic behavior and mass spectral data by comparison with those of reference substances. Chemicals added illegally were detected in 10 samples from 50 samples. Conclusion The method is sufficiently selective, sensitive and can be employed in the rapid determination of chemicals added illegally in anti-rheumatic traditional Chinese medicines and health products.

关 键 词：液质联用法 快速检测 抗风湿类 非法添加 

分 类 号：R917[医药卫生—药物分析学]