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Simultaneous quantification of 33 active components in Notopterygii Rhizoma et Radix using ultra high performance liquid chromatography with tandem mass spectrometry
Journal of Chromatography B ( IF 3 ) Pub Date : 2018-06-08 , DOI: 10.1016/j.jchromb.2018.06.006
Xiu-Wen Wu , You-Bo Zhang , Lei Zhang , Xiu-Wei Yang

A method of ultra high performance liquid chromatography with tandem mass spectrometry was developed for the simultaneous quantification of 33 active components including 26 coumarins and 7 phenolic acid esters in Notopterygii Rhizoma et Radix (NRR). Chromatographic separation was achieved on a Kinetex® C18 column (100 mm × 2.1 mm i.d.; 2.6 μm) with a gradient elution in 18 min. Electrospray ionization tandem mass spectrometric detection was conducted in the positive and negative ionization modes with multiple reaction monitoring. All of 33 analytes showed good linearity (R2 ≥ 0.9919) within the test range. The relative standard deviations of the precision, repeatability and stability were not exceeding 4.97%, and the recoveries were in the range of 85.37%–115.00%. The matrix effect on the response of target analyte was not obvious. The validated method was successfully applied to quantify the 33 components in ten batches of NRR samples. Quantitative results showed the coumarins and phenolic acid esters with large difference in level of content in the herb samples. Furthermore, hierarchical cluster analysis and principal component analysis were applied to classify and discriminate these samples. The variations of isoimperatorin, notopterol, bergamottin, nodakenin, phenethylferulate were suggested as important indicators of NRR quality. This work may serve for quality identification and comprehensive evaluation of NRR.



中文翻译:

使用串联质谱的超高效液相色谱法同时对Not药和板蓝根中的33种活性成分进行定量

开发了一种采用串联质谱的超高效液相色谱方法,用于同时定量Notopterygii Rhizoma et Radix(NRR)中的33种活性成分,包括26种香豆素和7种酚酸酯。在Kinetex®C 18色谱柱(100 mm×2.1 mm内径; 2.6μm)上进行色谱分离,并在18分钟内进行梯度洗脱。电喷雾电离串联质谱检测以正电离和负电离模式进行,并带有多个反应监控。33种分析物均显示出良好的线性(R 2 ≥0.9919)在测试范围内。精密度,重复性和稳定性的相对标准偏差不超过4.97%,回收率在85.37%–115.00%的范围内。基质对目标分析物响应的影响不明显。该验证方法已成功应用于十批NRR样品中的33种成分的定量分析。定量结果表明,香豆素和酚酸酯在草药样品中的含量水平差异很大。此外,应用层次聚类分析和主成分分析对这些样本进行分类和区分。异欧前胡素,异戊醇,佛手柑,诺达肯宁,阿魏酸苯乙酯的变化被认为是NRR质量的重要指标。这项工作可用于NRR的质量识别和综合评估。

更新日期:2018-06-08
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