干旱区生态环境知识资源中心(Arid): 超高效液相串联质谱法同时测定中成药中5-甲氧基补骨脂素,8-甲氧基补骨脂素和欧前胡素

Arid

	超高效液相串联质谱法同时测定中成药中5-甲氧基补骨脂素,8-甲氧基补骨脂素和欧前胡素
其他题名	Simultaneous determination of 5-methoxypsoralen,8-methoxypsoralen and imperatorin in duliang dropping pills by ultra performance liquid chromatography tandem mass spectrometry
	席海为 1; 马强 2; 王超 2; 白桦 2; 李强 1; 雷海民 1
来源期刊	分析试验室
ISSN	1000-0720
出版年	2010
卷号	29 期号:12 页码:98-101
中文摘要	建立了同时测定中成药都梁滴丸中5-甲氧基补骨脂素,8-甲氧基补骨脂素和欧前胡素的超高效液相-串联质谱检测方法.都梁滴丸以甲醇超声提取45 min,提取液稀释后经Waters Oasis HLB固相萃取小柱净化,采用WatersACQUITY UPLC BEHC18(50 mm*2.1 mm,1.7mum)色谱柱,以乙腈(A)和水(B)为流动相进行梯度洗脱.采用电喷雾电离正离子模式,多反应监测模式检测,以保留时间和离子比定性,外标法定量.方法的定量限8-甲氧基补骨脂素和5-甲氧基补骨脂素均为0.3 mg/kg;欧前胡素为0.75 mg/kg.3种化合物在25500mug/L范围内均呈线性,相关系数r>0.99.在高,中,低三种添加水平的平均回收率为82.0%107.4%日内精密度(RSD%)为1.1%12%
英文摘要	An analytical method based on ultra performance liquid chromatography tandem mass spectrometry has been developed for the determination of 5-Methoxypsoralen,8-Methoxypsoralen and Imperatorin.Duliang Dropping pills were extracted supersonically with methanol for 45 min,the extract was cleaned up by Oasis HLB solid phase extraction cartridge.After the chromatographic separation was performed on a Waters ACQUITY UPLC BEH C18 column(50 mm * 2.1 mm,1.7 mum),qualitative and quantitative analysis was carried out on ESI-MS/MS in the positive ion mode using multiple reaction monitoring.Identification was achieved by the retention time and the ion ratio,quantification was done by the external standard curve.The limits of quantification(LOQs) for 5-Methoxypsoralen,8-Methoxypsoralen and Imperatorin were 0.3mg/kg,0.3mg/kg and 0.75 mg/kg separately.All the linear ranges of three compounds were in the range of 25~500 mug/L,with correlations coefficient(r) more than 0.99.The mean recoveries at three spiked level were 82.0%~107.4%,with the relative standard deviations between 1.1% and 12%.The method is rapid,accurate,simple and adapts to the determination 5-Methoxypsoralen,8-Methoxypsoralen and Imperatorin in Chinese medicine
中文关键词	超高效液相色谱 ; 串联质谱 ; 固相萃取 ; 都梁滴丸 ; 甲氧基补骨脂素
英文关键词	Ultra performance liquid chromatography Tandem mass spectrometry Solid Phase Extract Duliang Dropping Pills Methoxypsoralens Imperatorin
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY ANALYTICAL
WOS研究方向	Chemistry
CSCD记录号	CSCD:4089464
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/224927
作者单位	1.北京中医药大学中药学院, 北京 100102, 中国; 2.中国检验检疫科学研究院, 北京 100123, 中国
推荐引用方式 GB/T 7714	席海为,马强,王超,等. 超高效液相串联质谱法同时测定中成药中5-甲氧基补骨脂素,8-甲氧基补骨脂素和欧前胡素[J],2010,29(12):98-101.
APA	席海为,马强,王超,白桦,李强,&雷海民.(2010).超高效液相串联质谱法同时测定中成药中5-甲氧基补骨脂素,8-甲氧基补骨脂素和欧前胡素.分析试验室,29(12),98-101.
MLA	席海为,et al."超高效液相串联质谱法同时测定中成药中5-甲氧基补骨脂素,8-甲氧基补骨脂素和欧前胡素".分析试验室 29.12(2010):98-101.