摘要
目的建立外用制剂（软膏和喷雾剂）中7种皮质激素的HPLC/ESI-MS-MS检测方法。方法选用Waters XTerra C18（2.1mm×150mm,3.5μm）反相色谱柱,流动相为乙腈-水（含0.1%甲酸）,梯度洗脱,流速为0.2mL·min^-1。采用电喷雾电离源液质联用仪分析鉴定,监测模式为多反应监测（MRM）。结果苯丙酸诺龙,丁酸氢化可的松,曲安奈德,氯氟舒松,醋酸氟轻松,醋酸地塞米松和丙酸倍氯米松的检出限分别是0.4,0.76,0.6,0.4,0.5,0.8,0.2ng,回收率为75%~90%,相对标准偏差为1.9%~8.6%。该方法可以对7种激素进行检测。结论该法特异性高,选择性强,灵敏度高,分析时间短,可应用于制剂和化妆品中激素的监测。
OBJECITVE To establish a HPLC/ESI-MS-MS method for the determination and identification of seven hormones in ointments and sprays. METHODS The separation was performed on a＇Waters XTerra C18 （2. 1 mm × 150 mm,3.5 μm） column with the Mobile phase consisting of acetonitrile-water （contains 0. 1% formic acid） by gradientelution, flow rate was 0.2 mL · min^-1 ; the mass spectrometer was equipped with ESI source and operated in positive ion mode using multiple reaction monitoring. RESULTS The limit of detection（LOD） was 0. 4,0. 76, 0. 6, 0.4, 0. 5,0. 8,0.2 ng for nandrolone phenylpropionate,hydrocortisone,halcinonidedcorten , triamcinolone, fluocinonide , dexamethasone acetate, beclomethasone, respectively. The recoveries ranged from 75 % to 90%, RSDs from 1.9% to 8.6%. CONCLUSION The method is sensitive, accurate, convenient and fast, which can meet the requirements for residues determination.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2007年第18期1431-1433,共3页
Chinese Pharmaceutical Journal
关键词
液质联用仪
激素
软膏和喷雾剂
测定
HPLC/ESI-MS-MS
hormones
ointment and spray
determination
