采用高效液相色谱法与电喷雾检测器联用控制 L-天冬氨酸和 L-丙氨酸中的杂质。
Control of impurities in L-aspartic acid and L-alanine by high-performance liquid chromatography coupled with a corona charged aerosol detector.
机构信息
University of Wuerzburg, Institute of Pharmacy and Food Chemistry, Am Hubland, 97074 Wuerzburg, Germany.
出版信息
J Chromatogr A. 2010 Jan 15;1217(3):294-301. doi: 10.1016/j.chroma.2009.11.036. Epub 2009 Nov 18.
In this study a reversed phase ion-pair high-performance liquid chromatography (HPLC) method using charged aerosol detection (CAD) was developed and fully validated for the pharmaceutical quality control of L-aspartic acid (Asp). With a slight modification, the method also allows the evaluation of related substances in L-alanine (Ala). The method enables simultaneous control of related amino acids and of possibly occurring organic acids contaminants. A minimum limit of quantification of 0.03% could be achieved for all occurring related substances. Moreover, the detector sensitivity of the CAD was compared with an evaporative light scattering detector (ELSD). Depending on the analyte the CAD was found to be 3.6-42 times more sensitive than the ELSD. The HPLC method was applied to the purity testing of 8 samples of pharmaceutical grade and reagent grade Asp and of 12 samples of Ala supplied by various manufacturers. Both substances were found to be of high purity (greater than 99.8% for Asp and greater than 99.9% for Ala). Malic acid and Ala were the major impurities in Asp. Asp and glutamic acid (Glu) were the only detectable impurities in Ala.
在这项研究中，建立了一种反相离子对高效液相色谱（HPLC）方法，并用带电气溶胶检测（CAD）进行了全面验证，用于 L-天冬氨酸（Asp）的药物质量控制。经过轻微修改，该方法还可以评估 L-丙氨酸（Ala）中的相关物质。该方法能够同时控制相关氨基酸和可能存在的有机酸污染物。对于所有出现的相关物质，最低定量限可达到 0.03%。此外，还比较了 CAD 和蒸发光散射检测器（ELSD）的检测器灵敏度。根据分析物的不同，CAD 的灵敏度比 ELSD 高 3.6-42 倍。该 HPLC 方法应用于纯度测试，测试了 8 个制药级和试剂级 Asp 样品和 12 个来自不同制造商的 Ala 样品。两种物质的纯度都很高（Asp 大于 99.8%，Ala 大于 99.9%）。苹果酸和 Ala 是 Asp 的主要杂质。Asp 和谷氨酸（Glu）是 Ala 中唯一可检测到的杂质。
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