Qualification of HSQC methods for quantitative composition of heparin and low molecular weight heparins

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• 作者：Lucio Mauri^a ; ¹ ; Giovanni Boccardi^a ; ¹ ; Giangiacomo Torri^a ; Michael Karfunkle^b ; Eleonora Macchi^a ; Laura Muzi^a ; David Keire^b ; ^{David.Keire@fda.hhs.gov} ; Marco Guerrini^a ; ^{guerrini@ronzoni.it}
• 关键词：Heparin ; Low molecular weight heparins ; Quantitative NMR ; Heteronuclear Single Quantum Correlation (HSQC) ; Robustness ; Method qualification
• 刊名：Journal of Pharmaceutical and Biomedical Analysis
• 出版年：2017
• 出版时间：20 March 2017
• 年：2017
• 卷：136
• 期：Complete
• 页码：92-105
• 全文大小：1907 K
• 卷排序：136

文摘

Robust heparin mono- and di-saccharide composition measurements are a key tests for ensuring drug quality. NMR HSQC data enables quick and detailed heparin compositional analysis with minimal sample treatment. A robustness investigation and method validation showed the NMR technique was suitable for pharmaceutical quality assessment purposes. Signal to noise measurements provided a metric for inclusion of peaks in composition analysis and for the proposal of a System Suitability Test. Important NMR factors for optimal performance were pulse sequence, relaxation delay and temperature control.