Electrochemical determination of emodin in acidic media by high-performance liquid chromatography and its application to Polygoni Multiflori Radix samples
Electrochemical determination of emodin in acidic media by high-performance liquid chromatography and its application to Polygoni Multiflori Radix samples
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DOI：
10.1007/s44211-022-00177-5
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发表时间：
2022-08
影响因子：
1.6
通讯作者：
Aya Shiozawa;Y. Kojima;Akira Kotani;K. Machida;Kazuhiro Yamamoto;H. Hakamata
中科院分区：
文献类型：
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作者：
Aya Shiozawa;Y. Kojima;Akira Kotani;K. Machida;Kazuhiro Yamamoto;H. Hakamata
与中性介质相比，大黄素在酸性介质中的电化学还原发生在较小的负电位。当大黄素在较低的负电势下进行电化学检测时，背景噪声的减少和专属性的提高有利于发展高效液相色谱-电化学检测方法(LC-ECD)。采用十八烷基硅胶色谱柱，乙腈-水(60：40，v/v)为流动相，流动相为含5 mmo1 L−1盐酸和10 mmo1 L−1高氯酸锂，外加电位为−=0.4 5V vs Ag/AgCl.在此最佳条件下，大黄素的检出限(信噪比，S/N = 3)为0.61gμ/L−1。将该体系用于何首乌样品中大黄素的测定，其他峰均未出现在与色谱峰相近的位置。样品中大黄素含量的相对标准偏差(RSD，n= 6)小于3.9%，加标回收率为92~106%。我们已经证明，我们的高效液相色谱-电子捕获检测器系统能够准确、准确、特异地测定PMR样品中的大黄素。
Electrochemical reduction of emodin under acidic media occurs at a less negative potential when compared with that under neutral media. When emodin is electrochemically detected at a less negative potential, a decrease in background noise and improvement in specificity benefit the development of high-performance liquid chromatography with electrochemical detection (HPLC-ECD) for its determination. HPLC-ECD was performed using an octadecyl silica column, acetonitrile–water (60:40, v/v) containing 5 mmol L−1hydrochloric acid and 10 mmol L−1lithium perchlorate, as a mobile phase, and an applied potential at − 0.4 V vs. Ag/AgCl. Under these optimal HPLC-ECD conditions, the detection limit (signal-to-noise ratio, S/N = 3) of emodin was 0.61 μg L−1. When this HPLC-ECD system was applied to the determination of emodin in Polygoni Multiflori Radix (PMR) samples, other peaks did not appear close to the emodin peak on a chromatogram. The emodin contents in PMR samples were determined with relative standard deviations (RSDs,n= 6) of less than 3.9%, and their recoveries ranged from 92 to 106%. We have shown that our HPLC-ECD system performed an accurate, precise, and specific determination of emodin in PMR samples.Graphical abstract