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比较 HPLC 法测定炮制前后乌头中毒性生物碱与总生物碱滴定法。

Comparison of a specific HPLC determination of toxic aconite alkaloids in processed Radix aconiti with a titration method of total alkaloids.

机构信息

Department of Pharmacognosy, University of Szeged, Szeged, Hungary.

出版信息

Pharm Biol. 2011 Oct;49(10):1097-101. doi: 10.3109/13880209.2011.595011.

Abstract

CONTEXT

In traditional Chinese medicine, Aconitum (Ranunculaceae) roots are only applied after processing. Nevertheless, several cases of poisoning by improperly processed aconite roots have been reported.

OBJECTIVE

The aim of this study was to develop a reliable analytical method to assess the amount of toxic aconite alkaloids in commercial aconite roots, and to compare this method with the commonly used total alkaloid content determination by titration.

MATERIALS AND METHODS

The content of mesaconitine, aconitine, and hypaconitine in 16 commercial samples of processed aconite roots was determined by an HPLC method and the total alkaloid content by indirect titration. Five samples were selected for in vivo toxicological investigation.

RESULTS

In most of the commercial samples, toxic alkaloids were not detectable, or only traces were found. In four samples, we could detect >0.04% toxic aconite alkaloids, the highest with a content of 0.16%. The results of HPLC analysis were compared with the results obtained by titration, and no correlation was found between the two methods. The in vivo results reassured the validity of the HPLC determination.

DISCUSSION AND CONCLUSION

Samples with mesaconitine, aconitine, and hypaconitine content below the HPLC detection limit still contained up to 0.2% alkaloids determined by titration. Since titration of alkaloids gives no information selectively on the aconitine-type alkaloid content and toxicity of aconite roots this method is not appropriate for safety assessment. The HPLC method developed by us provides a quick and reliable assessment of toxicity and should be considered as a purity test in pharmacopoeia monographs.

摘要

背景

在中医中,乌头(毛茛科)根仅在加工后使用。然而,已经报道了几起因不当加工乌头根而中毒的病例。

目的

本研究旨在开发一种可靠的分析方法来评估商业乌头根中有毒乌头生物碱的含量,并将该方法与常用的滴定法总生物碱含量测定进行比较。

材料和方法

采用 HPLC 法测定 16 份市售炮制乌头根中中乌头碱、乌头碱和次乌头碱的含量,并采用间接滴定法测定总生物碱含量。选择了 5 个样品进行体内毒理学研究。

结果

在大多数市售样品中,未检测到有毒生物碱,或仅检测到痕量。在 4 个样品中,我们可以检测到>0.04%的有毒乌头生物碱,最高含量为 0.16%。HPLC 分析结果与滴定法结果进行了比较,两种方法之间没有相关性。体内结果证实了 HPLC 测定的有效性。

讨论与结论

HPLC 检测限以下的样品中仍含有高达 0.2%的通过滴定法测定的生物碱。由于生物碱的滴定法不能选择性地提供乌头碱型生物碱含量和乌头根毒性的信息,因此该方法不适合安全性评估。我们开发的 HPLC 方法为毒性和应考虑作为药典专论中纯度测试的快速可靠评估提供了快速可靠的评估。

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