Abstract：
:For the compendial related substances test of l-aspartic acid (Asp) and glycine (Gly), two separate reversed-phase ion-pair high-performance liquid chromatography methods coupled with charged aerosol and ultraviolet detection were developed. Separation of all putative impurities, in particular of the related carboxylic and amino acids, was achieved using volatile perfluorocarboxylic acids as ion-pairing reagents on a polar embedded C18 stationary phase. It was shown that an adjustment of the evaporation temperature of the charged aerosol detector (CAD) was an efficient strategy for meeting the required quantitation limits, when dealing with non-volatile analytes. It was also demonstrated that the usage of a two detector setup can be beneficial for extending the detection range and providing accurate quantitation of low level impurities (LOQs from 5 to 50 ng on column). Both methods were validated with accordance to ICH guideline Q2(R1) assessing specificity, linearity, accuracy, precision, and robustness. Several batches of Asp and Gly were tested for related substances using the developed methods. The purity of each sample was higher than 99.7 %. Coupled charged aerosol and UV detection proved to be a more simple, robust and selective alternative to established derivatization procedures such as the Amino-Acid-Analyser (AAA) for the impurity profiling of amino acids, and should thus be considered for implementation into pharmacopoeial monographs in the future.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Pawellek R,Schilling K,Holzgrabe Udoi
10.1016/j.jpba.2020.113149subject
Has Abstractpub_date
2020-05-10 00:00:00pages
113149eissn
0731-7085issn
1873-264Xpii
S0731-7085(19)32911-5journal_volume
183pub_type
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
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