开发和验证用于多酚定量评估的色谱-质谱技术

N. Popov, A. A. Antipina, S. V. Savintsev, V. Balabanyan
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摘要

简介。多酚是一类天然长链异戊烯醇,是直接参与细胞膜糖蛋白合成的天然生物调节剂。它们的保肝活性已得到证实,其他类型的药理作用也已为人所知,这也是人们对这些物质作为一种有前途的医药产品产生浓厚兴趣的原因。确定提取物中多酚的总含量并非易事,其中包括设计和实施准确的可重复分析方法,这些方法随后将用于标准化。开发并验证用于鉴定和定量评估多酚的色谱-质谱技术。使用高效液相色谱仪 Agilent 1260 Infinity II(安捷伦科技,США)对多烯醇进行色谱分离;甲醇、正己烷、丙醇-2 和乙酸铵水溶液的混合物作为梯度洗脱液。使用 AB Sciex QTrap® 3200MD(AB Sciex 私人有限公司,新加坡)三重四极杆质谱仪作为检测器,对多酚加合物进行登记。确定了色谱分离和检测多酚的条件。对所开发技术的以下特性进行了验证:特异性、检测限、定量限、线性、准确性、精密度、适用范围和稳定性。所开发的技术今后可用于评估药物产品或医药物质中多酚的含量。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Development and validation of the chromatography-mass spectrometry technique for polyprenols quantitative assessment
Introduction. Polyprenols are known as a class of natural long-chain isoprenoid alcohols, which are natural bioregulators that directly participate in the synthesis of cell membrane glycoproteins. Their hepatoprotective activity is proven, as well other types of their pharmacological effects are known, which is the reason of significant interest in these substances as a promising medicinal product. It is non-trivial task to determine the sum of polyprenols in extracts as include design and implementation of accurate reproducible analytical methods, which will subsequently be used in standardization.Aim. Development and validation of the chromatographic-mass spectrometric technique for polyprenols identification and their quantitative assessment.Materials and methods. Chromatographic separation of polyprenols was performed by using an HPLC Agilent 1260 Infinity II (Agilent Technologies, США); with the mixture of methanol, n-hexane, propanol-2, and aqueous ammonium acetate solution as eluent in gradient mode. An AB Sciex QTrap® 3200MD (AB Sciex Pte. Ltd., Singapore) triple quadrupole mass spectrometer was used as a detector, with the registration of polyprenols adducts.Results and discussion. The conditions for chromatographic separation and detection of polyprenols were identified. The developed technique was validated for the following characteristics: specificity, limit of detection, limit of quantification, linearity, accuracy, precision, range of application, and stability.Conclusion. It was determined the content of polyprenols in the substance recieved from Ginkgo biloba L. and Picea abies L. The developed technique can be used in the future to assess the content of polyprenols in drug products or pharmaceutical substances.
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