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采用超高效液相色谱-串联质谱法同时测定传统草药处方“归命风湿丸”中的 14 种标记化合物。

Simultaneous Determination of Fourteen Marker Compounds in the Traditional Herbal Prescription, Geumgwesingihwan, Using Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry.

机构信息

KM Science Research Division, Korea Institute of Oriental Medicine, Daejeon 34054, Korea.

KM Convergence Research Division, Korea Institute of Oriental Medicine, Daejeon 34054, Korea.

出版信息

Molecules. 2022 Jun 17;27(12):3890. doi: 10.3390/molecules27123890.

DOI:10.3390/molecules27123890
PMID:35745012
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9227478/
Abstract

Geumgwesingihwan (GSH) is a traditional herbal prescription composed of eight medicinal herbs: (Gaertn.) DC., Thunb., Siebold and Zucc., Wolf, Andrews, subsp. (Sam.) Sam., Blume, and L. This study developed and validated an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method in the multiple reaction monitoring (MRM) mode for simultaneous determination of 14 compounds (allantoin, gallic acid, 5-(hydroxymethyl)furfural, geniposidic acid, oxypaeoniflorin, loganin, geniposide, paeoniflorin, ecdysterone, verbascoside, cornuside, benzoylpaeoniflorin, paeonol, and alisol B acetate) in GSH. The chromatographic separation of all marker analytes was carried out on an Acquity UPLC BEH C column (100 mm × 2.1 mm, 1.7 µm) using gradient elution of a mobile phase of distilled water-acetonitrile containing 0.1% acetic acid. The newly established UPLC-MS/MS MRM method was validated by evaluating the linearity, the limits of detection and quantification, recovery, and precision. All markers were detected at concentrations of 6.94-4126.28 mg/kg. In addition, the recovery was 76.65-119.49% and the relative standard deviation value of the precision was 0.19-9.91%. The newly developed and validated UPLC-MS/MS assay will provide useful information for quality assessment of GSH.

摘要

归芪四物汤(GSH)是一种由八种草药组成的传统草药处方:(Gaertn.)DC.、Thunb.、Siebold 和 Zucc.、Wolf、Andrews、subsp.(Sam.)Sam.、Blume 和 L.。本研究开发并验证了一种超高效液相色谱-串联质谱(UPLC-MS/MS)方法,采用多重反应监测(MRM)模式,可同时测定 14 种化合物(尿囊素、没食子酸、5-(羟甲基)糠醛、京尼平酸、氧化芍药苷、马钱苷酸、栀子苷、芍药苷、蜕皮甾酮、毛蕊花糖苷、小檗碱、苯甲酰芍药苷、丹皮酚和乙酸泽泻醇 B)。所有标记分析物的色谱分离均在 Acquity UPLC BEH C 柱(100mm×2.1mm,1.7µm)上进行,采用梯度洗脱,流动相为含 0.1%乙酸的蒸馏水-乙腈。新建立的 UPLC-MS/MS MRM 方法通过评价线性、检测限和定量限、回收率和精密度进行了验证。所有标志物的浓度均在 6.94-4126.28mg/kg 之间。此外,回收率为 76.65-119.49%,精密度的相对标准偏差值为 0.19-9.91%。新开发和验证的 UPLC-MS/MS 测定法将为 GSH 的质量评估提供有用信息。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a95/9227478/97079e01747b/molecules-27-03890-g001a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a95/9227478/97079e01747b/molecules-27-03890-g001a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a95/9227478/97079e01747b/molecules-27-03890-g001a.jpg

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