LC-MS/MS法检测皮肤科中药制剂中掺加的8种糖皮质激素  

Detection of eight glucocorticosteroids adulterated in traditional Chinese medicine preparations for dermatology by LC-MS/MS

作　　者：叶林虎 王丽莎[2] 贺梅 常琪[2] 

机构地区：[1]毕节市第一人民医院药剂科,贵州毕节551700 [2]中国医学科学院-北京协和医学院药用植物研究所,北京100193

出　　处：《中成药》2016年第12期2626-2631,共6页Chinese Traditional Patent Medicine

基　　金：毕节市科技局资助项目(毕科合字[2015]51;62);贵州省科学技术基金项目(黔科合J字[2015]2004);"重大新药创制"科技重大专项(2012ZX09301002-001)

摘　　要：目的建立液相色谱-串联质谱（LC-MS/MS）法检测9种皮肤科中药制剂中掺加的8种糖皮质激素（倍氯米松、醋酸泼尼松、醋酸氟轻松、甲基泼尼松龙醋酸酯、可的松、泼尼松龙、氢化可的松、曲安奈德）。方法 12批样品甲醇提取液的分析均采用Agilent C18色谱柱（50 mm×20 mm,5μm）;流动相乙腈-水,梯度洗脱;体积流量0.4m L/min;柱温40℃。结果 8种糖皮质激素在各自范围内均呈现出良好的线性关系,最低检测限0.5~1.0 ng/m L,最低定量限1.0~4.0 ng/m L,加样回收率88.2%~112.4%,RSD 0.6%~13.1%。除醋酸氟轻松和曲安奈德外,各糖皮质激素均被不同程度地掺加进9批样品中（样品E、G、H除外）。结论该方法简便快捷,准确灵敏,可用于检测皮肤科中药制剂中掺加的糖皮质激素。AIM To establish a liquid chromatography-tandem mass spectrometry（ LC-MS / MS） method for detecting eight glucocorticosteroids（ beclomethasone,prednisone acetate,fluocinonide,methylprednisolone acetate,cortisone,prednisolone,hydrocortisone and triamcinolone acetonide） adulterated in nine kinds of traditional Chinese medicine preparations for dermatology. METHODS The analyses of twelve batches of samples（ A-I） ＇methanol extracts were performed on a 40 ℃ thermostastic Agilent C18column（ 50 mm × 20 mm,5 μm）,with the mobile phase comprising of acetonitrile-water flowing at 0. 4 m L / min in a gradient elution manner. RESULTS Eight glucocorticosteroids showed good linear relationships within their own ranges,whose limits of detection and limits of quantitative were 0. 5- 1. 0 ng / m L and 1. 0- 4. 0 ng / m L,respectively. And their recoveries were88. 2%- 112. 4% with the RSDs of 0. 6%- 13. 1%. Various glucocorticosteroids,except fluocinonide and triamcinolone acetonide,were adulterated in nine batches of samples（ except samples E,G and H） to different degrees.CONCLUSION This method is simple and accurate with sensitive,which can be used for detecting glucocorticosteroids adulterated in traditional Chinese medicine preparations for dermatology

关 键 词：皮肤科中药制剂 糖皮质激素 LC-MS/MS 

分 类 号：R284.1[医药卫生—中药学]