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口服紫锥菊提取物后,采用超高效液相色谱-串联质谱法同时测定大鼠血浆中四种酚类化合物并进行药代动力学研究。

Simultaneous determination and pharmacokinetic study of four phenol compounds in rat plasma by ultra-high performance liquid chromatography with tandem mass spectrometry after oral administration of Echinacea purpurea extract.

作者信息

Gan Chunli, Liu Lu, Du Yan, Wang Liqian, Gao Mingjie, Wu Lijun, Yang Chunjuan

机构信息

College of Pharmacy, Harbin Medical University, Nangang District, Harbin, China.

出版信息

J Sep Sci. 2016 May;39(9):1628-37. doi: 10.1002/jssc.201600051. Epub 2016 Apr 19.

Abstract

A rapid and sensitive assay based on ultra-high performance liquid chromatography with electrospray ionization tandem mass spectrometry was established and validated for the simultaneous determination of cichoric acid, chlorogenic acid, quinic acid, and caffeic acid in rat plasma after oral administration of Echinacea purpurea extract using butylparaben as the internal standard. Samples were pretreated by liquid-liquid extraction with ethyl acetate. The separations for analytes were performed on an ACQUITY UPLC HSS C18 column (1.8 μm 2.1 × 100 mm) using a gradient elution program with acetonitrile/10 mM ammonium acetate (pH 5.6) at a flow rate of 0.3 mL/min. The analytes were detected in multiple reaction monitoring mode with negative electrospray ionization. The lower limit of quantification of each analyte was not higher than 10.85 ng/mL. The relative standard deviation of the intraday and interday precisions was less than 14.69%. The relative errors of accuracies were in the range of -13.80 to 14.91%. The mean recoveries for extraction recovery and matrix effect were higher than 80.79 and 89.98%, respectively. The method validation results demonstrated that the proposed method was sensitive, specific, and reliable, which was successfully applied to the pharmacokinetic study of four components after oral administration of Echinacea purpurea extract.

摘要

建立了一种基于超高效液相色谱-电喷雾电离串联质谱的快速灵敏分析方法,以对羟基苯甲酸丁酯为内标,用于同时测定大鼠口服紫锥菊提取物后血浆中的紫草酸、绿原酸、奎尼酸和咖啡酸。样品采用乙酸乙酯液-液萃取进行预处理。分析物在ACQUITY UPLC HSS C18柱(1.8μm,2.1×100mm)上进行分离,使用乙腈/10mM乙酸铵(pH 5.6)的梯度洗脱程序,流速为0.3mL/min。分析物在负电喷雾电离的多反应监测模式下进行检测。各分析物的定量下限均不高于10.85ng/mL。日内和日间精密度的相对标准偏差均小于14.69%。准确度的相对误差在-13.80%至14.91%范围内。萃取回收率和基质效应的平均回收率分别高于80.79%和89.98%。方法验证结果表明,该方法灵敏、特异且可靠,已成功应用于紫锥菊提取物口服给药后四种成分的药代动力学研究。

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