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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Pattern profiling of the herbal preparation picroliv using liquid chromatography-tandem mass spectrometry
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Pattern profiling of the herbal preparation picroliv using liquid chromatography-tandem mass spectrometry

机译:液相色谱-串联质谱法对中草药制剂吡咯利夫进行模式分析

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At present, the construction of chromatographic fingerprints of complex herbal preparations in combination with mass spectrometry plays an important role in their development and standardization as potential therapeutic agents. Picroliv, an extract from roots and rhizomes of Picrorhiza kurroa, is a herbal hepatoprotective developed by CDRI. We report for the first time pattern profiling of various constituents of picroliv along with a precise and accurate method to estimate relative concentration of major components in the preparation by liquid chromatography-tandem mass spectrometry. In total, 27 components could be detected in multiple reaction monitoring (MRM) mode out of which fourteen could be quantified in terms of their relative concentration. Seven components were structurally correlated and confirmed based on the fragmentation pattern and information available in literature. The detection was carried out using MRM in negative ionization mode with analytes quantified from the summed total ion value of their most intense molecular ion transitions. The separation of various components was achieved using a gradient elution on RP-18 column with acetonitrile and Milli-Q water as mobile phase at a flow rate of 1.0 ml/min. The method was validated in terms of linearity, accuracy and precision (within- and between-assay variation) for 5 days. Linearity range was different for various components depending upon their sensitivity and abundance in the herbal preparation. Within- and between-assay accuracy (%bias) and precision (%R.S.D.) were within acceptable limits. The method was successfully applied to detect and determine relative concentrations of various components in two different batches of picroliv. (C) 2004 Elsevier B.V. All rights reserved.
机译:目前,复杂草药制剂与质谱联用的色谱指纹图谱的构建在其作为潜在治疗剂的开发和标准化中起着重要作用。 Picroliv是从Picrorhiza kurroa的根和根茎中提取的提取物,是CDRI开发的草药保肝剂。我们首次报告了吡咯利夫的各种成分的模式特征分析,以及通过液相色谱-串联质谱法估算制剂中主要成分的相对浓度的精确方法。总共可以在多反应监测(MRM)模式下检测到27种成分,其中14种可以根据它们的相对浓度进行定量。根据片段化模式和文献中提供的信息,七个组分在结构上相关并得到确认。使用MRM以负电离模式进行检测,分析物根据其最强分子离子跃迁的总离子值求和。使用RP-18色谱柱,以乙腈和Milli-Q水作为流动相,以1.0 ml / min的流速进行梯度洗脱,可实现各种组分的分离。该方法在线性,准确性和精密度(批内和批间差异)方面进行了5天的验证。各种成分的线性范围不同,这取决于它们在草药制品中的敏感性和丰度。测定内和测定间准确度(%bias)和精密度(%R.S.D。)在可接受的范围内。该方法已成功应用于检测和确定两个不同批次的吡咯利夫中各种成分的相对浓度。 (C)2004 Elsevier B.V.保留所有权利。

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