Improved liquid chromatographic method with pulsed electrochemical detection for the analysis of gentamicin
Improved liquid chromatographic method with pulsed electrochemical detection for the analysis of gentamicin
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DOI：
10.1016/j.chroma.2007.12.041
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发表时间：
2008-05-02
影响因子：
4.1
通讯作者：
Adams, Erwin
中科院分区：
文献类型：
--
作者：
Manyanga, Vicky;Kreft, Katjusa;Adams, Erwin
欧洲药典（Ph. Eur.）规定的庆大霉素成分及有关物质的正式测定方法是液相色谱结合脉冲电化学检测（LC-PED）。然而，该方法使用聚合物固定相，其对庆大霉素主要成分的分离效率相当低。此外，流动相含有大量的非挥发性盐：硫酸钠和辛烷磺酸钠。通过对比研究，我们使用反相C18色谱柱（C18, 250 × 4.6 mm ID， 110埃，5 μ m），在35℃下保持，流动相中含有挥发性离子配对剂：三氟乙酸（TFA）和五氟丙酸（PFPA），对最高效的LC-PED方法进行了评估和验证。除对庆大霉素主要成分及其相关物质有选择性外，该方法重复性好，线性好，稳健性好。它也适用于更大数量的C18列。(c) 2007 Elsevier B.V.版权所有
The official method for the determination of the composition and related substances of gentamicin prescribed by the European Pharmacopoeia (Ph. Eur.) is liquid chromatography combined with pulsed electrochemical detection (LC-PED). However, this method utilizes a polymer stationary phase which shows rather low efficiency towards the separation of the main gentamicin components. Moreover, the mobile phase contains a lot of non volatile salts: sodium sulphate and sodium octanesulphonate. Following a comparative study, the most performant LC-PED method has been evaluated and validated using a reversed phase C18 column (C18, 250 x 4.6 mm ID, 110 angstrom, 5 mu m) kept at 35 degrees C with a mobile phase containing volatile ion pairing agents: trifluoroacetic acetic acid (TFA) and pentafluoropropionic acid (PFPA). In addition to the selectivity of the main gentamicin components and its related substances, the method is repeatable, linear and proves to be robust. It is also applicable to a wider number of C18 columns. (c) 2007 Elsevier B.V. All rights reserved.