【作者】 王莹； 袁瑾； 安叡； 王新宏；

【Author】 WANG Ying,YUAN Jin,AN Rui,WANG Xin-hong Department of Chemistry,College of Pharmacy,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China

【机构】 上海中医药大学中药学院化学教研室；

【摘要】 目的:研究异黄酮类成分葛根素（puerarin,PUR）、大豆苷元（daidzein,DDE）和黄酮类成分黄芩苷（baicalin,BCL）、汉黄芩苷（wogonoside,WGS）的液相色谱串联质谱（LC-MS/MS）检测方法,为开展中药复方葛根芩连汤提取物的药代动力学研究,建立灵敏可靠的血浆样品的定量分析方法。方法:血浆样品酸化后经乙酸乙酯提取浓缩,液相色谱分离[Waters C₁₈柱（3μm,2.1 mm×100 mm）柱,流动相乙腈-水（0.02%的甲酸）梯度洗脱,流速0.3 mL/min],电喷雾离子化三重四极杆串联质谱正离子多反应监测模式（MRM）检测,离子反应分别为m/z 417.1→m/z 399.1（PUR）、m/z 255.2→m/z 199.0（DDE）、m/z 447.1→m/z 271.0（BCL）、m/z 461.1→m/z 285.1（WGS）和内标物柚皮苷m/z581.4→m/z 273.0（Naringin,NRG）。结果:PUR,DDE和BCL,WGS的线性范围在6～4140 ng/mL之间,最低定量浓度为6 ng/mL;PUR,BCL和WGS的回收率>60%;DDE的回收率>50%。日内、日间RSD皆小于15%（n=5）。结论:成功建立了能够灵敏可靠地测定大鼠血浆样品中四种化合物浓度的分析方法,此方法能够用于葛根芩连提取物的药代动力学研究。更多还原

【Abstract】 AIM:To develop a sensitive and accurate liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for the measurement of puerarin,daidzein,baicalin and wogonoside in supporting the pharmacokinetic evaluation of GegenQinlian Decoction extract.METHODS:Plasma samples were extracted by ethyl acetate after acidification and separated on an Waters C18 column(100 mm×2.1 mm,3μm) with a mobile phase of acetonitrile-water-formic acid(0.02%) at a flow rate of 0.3 mL/min.LC-MS/MS detection was made with an electrospray positive ionization(ESI) and selected reaction monitoring(SRM).The transitions selected for quantitation were m/z 417.1→m/z 399.1(PUR)、m/z 255.2→m/z 199.0(DDE)、m/z 447.1→m/z 271.0(BCL)、m/z 461.1→m/z 285.1(WGS) and m/z 581.4→m/z 273.0(Naringin,I.S.).RESULTS:The calibration curve was linear over the concentration rang of 6 to 4140 ng/mL. The limit of quantitation was 6 ng/mL.The recovery was over 60% for PUR,BCL and WGS,and DDE was over 50%.Within-batch and between-batch RSD less than 15%(n=5).CONCLUSION:The established LC-MS/MS method is validated to be specific,accurate and sensitive for the pharmacokinetic study of four bioactive compounds of GegenQinlian decoction(GQD) extract in rats.更多还原