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作 者:秦建平[1,2] 吴建雄[1,2] 李艳静[1,2] 王雪[1,2] 李家春[1,2] 萧伟[1,2]
机构地区:[1]江苏康缘药业股份有限公司,连云港222001 [2]中药制药过程新技术国家重点实验室,连云港222001
出 处:《药物分析杂志》2014年第5期819-823,共5页Chinese Journal of Pharmaceutical Analysis
基 金:国家科技部重大新药创制"子宫内膜异位症首选用药-散结镇痛胶囊大品种技术改造"(项目编号:2011ZX09201-201-20)
摘 要:目的:建立一种可以快速鉴定龙血竭中5个酚酸类成分的方法。方法:采用实时直接分析(DART)离子源结合四极杆串联飞行时间质谱(Q-TOF-MS),氦气流速为3.1 L·min-1,气体温度为250℃,样品传输速度为0.2 mm·s-1。Agilent6538 Q-TOF毛细管电压为1 kV,RF电压为250 V,一级质谱扫描质荷比范围m/z 50~800,二级质谱扫描质荷比范围m/z30~500,碰撞能量为25 V。结果:通过对照品与样品的一级、二级质谱图对比快速鉴定了样品中5个化学成分,分别为龙血素A、龙血素B、7,4’-二羟基黄酮、白藜芦醇和紫檀茋。结论:本法经过方法学验证,可用于快速分析鉴定龙血竭中的酚酸类成分。Objective: To establish a rapid method for identification of 5 phenolic compounds in resina draconis. Methods: Direct analysis in real time ionization source( DART) coupled with quadrupole time-of-flight tandem mass spectrometry( DART / Q-TOF-MS) was performed for direct analysis of phenolic compounds. The flow rate of He was set at 3. 1 L·min-1. The temperature of carry gas of DART was 250 ℃. The sample delivery rate was 0. 2 mm·s-1. The capillary voltage was kept at 1 kV. The RF voltage was kept at 250 V. The MS scan range was m / z 50-800. The collision energy was 25 V. Results: Based on accurate mass measurements,and the elemental compositions of the product ions and fragmentation patterns of reference compounds,five components,including loureirin A,loureirin B,7,4'-dihydroxy flavone,resveratrol and pterostilbene,were identified in resina draconis. Conclusion: The DART Q-TOF MS method was validated,which can be used for rapid identification and characterization of phenolic compounds in resina draconis.
关 键 词:龙血竭 龙血素A 龙血素B 7 4’-二羟基黄酮 白藜芦醇 紫檀茋 直接实时分析 离子源结合 四极杆串联飞行时间质谱 快速鉴别
分 类 号:R917[医药卫生—药物分析学]
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