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基于超高效液相色谱-四极杆-轨道阱质谱联用仪和超高效液相色谱-三重四极杆串联质谱联用仪对沙药汤中植物化学成分的定性和定量分析

Qualitative and Quantitative Analysis of Phytochemicals in Sayeok-Tang via UPLC-Q-Orbitrap-MS and UPLC-TQ-MS/MS.

作者信息

Kim Yu Jin, Jang Seol, Hwang Youn-Hwan

机构信息

KM Convergence Research Division, Korea Institute of Oriental Medicine, 1672 Yuseong-daero, Yuseong-gu, Daejeon 34054, Republic of Korea.

出版信息

Pharmaceuticals (Basel). 2024 Aug 27;17(9):1130. doi: 10.3390/ph17091130.

Abstract

Sayeok-tang (SYT) is a traditional herbal formula comprising three medicinal herbs: , , and . Several studies have employed liquid chromatography-mass spectrometry (LC-MS) to qualitatively analyze the components and metabolites of SYT in vitro and in vivo; however, studies on quantitative analysis of SYT, which is important for quality control, are absent or limited to only a few components. In this study, ultrahigh-performance liquid chromatography coupled with quadrupole (UPLC-Q)-Orbitrap-MS was used to screen the phytochemicals of SYT, revealing a total of 42 compounds. Among them, 24 compounds were simultaneously quantified within 20 min via UPLC-TQ-MS/MS in the multiple reaction monitoring mode. The developed analytical method was validated for its linearity ( ≥ 0.9992), precision (0.36-2.96%), accuracy (-6.52-4.64%), and recovery (94.39-119.07%) for all analytes, exhibiting acceptable results. The validated method was applied in the analysis of SYT extracts, and the 24 compounds were quantified in the range of 0.004-6.882 mg/g (CV ≤ 3.746%). Among them, liquiritin apioside (6.870-6.933 mg/g), glycyrrhizic acid (5.418-5.540 mg/g), and liquiritin (1.303-1.331 mg/g) from were identified as the relatively abundant compounds. The presented validated analytical method is highly promising for the comprehensive quality control of SYT, offering fast, highly sensitive, and reliable analysis.

摘要

芍药汤(SYT)是一种由三种草药组成的传统中药配方:芍药、甘草和大黄。多项研究已采用液相色谱-质谱联用(LC-MS)技术对芍药汤在体外和体内的成分及代谢产物进行定性分析;然而,对于芍药汤质量控制至关重要的定量分析研究却缺失或仅局限于少数几种成分。在本研究中,采用超高效液相色谱-四极杆(UPLC-Q)-轨道阱质谱联用技术筛选芍药汤的植物化学成分,共鉴定出42种化合物。其中,通过UPLC-TQ-MS/MS在多反应监测模式下于20分钟内同时对24种化合物进行了定量分析。所建立的分析方法在所有分析物的线性(r≥0.9992)、精密度(0.36 - 2.96%)、准确度(-6.52 - 4.64%)和回收率(94.39 - 119.07%)方面均得到验证,结果令人满意。经验证的方法应用于芍药汤提取物的分析,24种化合物的定量范围为0.004 - 6.882 mg/g(CV≤3.746%)。其中,来自甘草的甘草苷元芹菜糖苷(6.870 - 6.933 mg/g)、甘草酸(5.418 - 5.540 mg/g)和甘草苷(1.303 - 1.331 mg/g)被确定为相对含量较高的化合物。所提出的经验证分析方法对于芍药汤的全面质量控制极具前景,可提供快速、高灵敏度且可靠的分析。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4be4/11435331/6f414a739897/pharmaceuticals-17-01130-g001.jpg

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