摘要
建立了白芷中欧前胡素,异欧前胡素和氧化前胡素的液相色谱-串联质谱分析法。白芷提取液经Waters XTerra-C18(150mm×3.9 mm,5μm)色谱柱分离,以1mmol/L乙酸铵溶液和乙腈为流动相进行洗脱,以电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,外标法定量。欧前胡素,异欧前胡素和氧化前胡素分别在0.05~10μg/mL,0.05~13μg/mL和0.1~120μg/mL范围内呈线性相关,相关系数(r)分别为0.9993,0.9991和0.9994,检出限分别为30,30和50 ng/mL,平均加标回收率为100.1%,99.4%和98.4%,相对标准偏差分别为2.2%,2.6%和2.8%(ρ=0.5μg/mL,n=6),该法可以满足同时检测白芷中欧前胡素,异欧前胡素和氧化前胡素的需求。
A liquid chromatography-tandem mass spectrometric(LC/MS/MS) method was developed for the determination of three coumarins in radix angelicae dahuricae.The standard samples were diluted and dissolved with methnol.The separation was performed on a Waters XTerra-C18 column by using elution with 1 mmol/L ammonium acetate solution and acetonitrile.The samples were determined by electrospray ionization-tandem mass spectrometry in positive mode,quantified by external standard method.The calibration curves of imperatorin,isoimperatorin and oxypeucedanin show good linearity in the concentration ranges of 0.05-10μg/mL,0.05-13μg/mL and 0.1-120μg/mL with correlation coefficients of 0.9993,0.9991 and 0.9994,respectively,and the limits of detection are 30,30 and 50 ng/mL.The recoveries of the method are 100.1%,99.4% and 98.4%.The relative standard deviation are 2.2%,2.6% and 2.8%(c=0.5μg/mL,n=6).The method can meet the requirement for the determination of imperatorin,isoimperatorin and oxypeucedanin in radix angelicae dahuricae and other drug related products.
出处
《分析试验室》
CAS
CSCD
北大核心
2012年第5期104-108,共5页
Chinese Journal of Analysis Laboratory
关键词
液相色谱-串联质谱
欧前胡素
异欧前胡素
氧化前胡素
香豆素
白芷
Liquid chromatography-tandem mass spectrometry(LC/MS/MS)
Imperatorin
Isoimperatorin
Oxypeucedanin
Radix angelicae dahuricae
Coumarin