KM Science Research Division, Korea Institute of Oriental Medicine, Daejeon 34054, Korea.
KM Convergence Research Division, Korea Institute of Oriental Medicine, Daejeon 34054, Korea.
Molecules. 2022 Jun 17;27(12):3890. doi: 10.3390/molecules27123890.
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.
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。