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建立并验证 SPE-HPLC 法测定鼠李科巴戟天中大黄素、大黄酚、大黄酸和大黄素甲醚的含量

Development and Validation of a SPE-HPLC Method for Quantification of Rhein, Emodin, Chrysophanol and Physcion in Rhamnus petiolaris Boiss. & Balansa.

机构信息

Department of Analytical Chemistry, Faculty of Pharmacy, Istanbul University, 34116 Istanbul, Türkiye.

出版信息

J Chromatogr Sci. 2024 Nov 1;62(9):872-877. doi: 10.1093/chromsci/bmad053.

DOI:10.1093/chromsci/bmad053
PMID:37501520
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC11530379/
Abstract

Anthraquinones exhibit a significant group of natural and synthetic quinone derivatives because of their biological activities and industrial applications. Rhamnaceae is one of the families known to contain different kinds of anthraquinones. In this study, it was aimed to quantify rhein, emodin, chrysophanol and physcion in fruits of Rhamnus petiolaris Boiss. & Balansa belonging to Rhamnaceae by solid phase extraction and high performance liquid chromatography with ultraviolet detection. The anthraquinones were separated using a C18 analytical column. Gradient elution was performed using a mobile phase consisted of 0.1% o-phosphoric acid solution and methanol. Analytes were detected at 254 nm. Calibration curves were prepared in the range of 0.25-5.00 μg/mL for rhein, chrysophanol, physcion, 1.00-50.00 μg/mL for emodin. Limits of detection and quantification were between 0.07-0.11 and 0.20-0.34 μg/mL, respectively. Relative standard deviations were ≤ 5.78% in repeatability and intermediate precision studies. Accuracy was determined as relative mean error (8.17-12.06%). Extraction was achieved by maceration with acetone and ethanol, followed by hydrophilic-lipophilic balance solid phase extraction. Recoveries were between 96.2 and 109.6%. The developed and validated method was successfully performed to quantify rhein, emodin, chrysophanol and physcion in R. petiolaris fruit extracts. Only physcion was not detected above limit of detection.

摘要

蒽醌类化合物因其生物活性和工业应用而显示出显著的天然和合成醌衍生物群体。鼠李科是已知含有不同种类蒽醌类化合物的科之一。在这项研究中,目的是通过固相萃取和高效液相色谱法与紫外检测定量测定属于鼠李科的 Rhamnus petiolaris Boiss. & Balansa 果实中的大黄酸、大黄素、大黄酚和大黄素甲醚。蒽醌类化合物使用 C18 分析柱分离。使用由 0.1%o-磷酸溶液和甲醇组成的流动相进行梯度洗脱。在 254nm 处检测分析物。为大黄酸、大黄酚、大黄素甲醚分别在 0.25-5.00μg/mL 范围内,大黄素在 1.00-50.00μg/mL 范围内制备校准曲线。检测限和定量限分别为 0.07-0.11μg/mL 和 0.20-0.34μg/mL。重复性和中间精密度研究中的相对标准偏差均≤5.78%。准确度以相对平均误差(8.17-12.06%)确定。通过丙酮和乙醇的浸提、亲水-亲脂平衡固相萃取来进行提取。回收率在 96.2%至 109.6%之间。所建立和验证的方法成功地用于定量测定 R. petiolaris 果实提取物中的大黄酸、大黄素、大黄酚和大黄素甲醚。只有大黄素甲醚未检出,低于检测限。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/222c/11530379/166bc317d238/bmad053f4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/222c/11530379/279f0138f37f/bmad053f1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/222c/11530379/6ef5d2f9686f/bmad053f2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/222c/11530379/c4bfe603614a/bmad053f3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/222c/11530379/166bc317d238/bmad053f4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/222c/11530379/279f0138f37f/bmad053f1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/222c/11530379/6ef5d2f9686f/bmad053f2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/222c/11530379/c4bfe603614a/bmad053f3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/222c/11530379/166bc317d238/bmad053f4.jpg

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