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KMID : 0043320160390070937
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Archives of Pharmacal Research
2016 Volume.39 No. 7 p.937 ~ p.945
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Determination of process-related impurities in N-acetylglucosamine prepared by chemical and enzymatic methods: structural elucidation and quantification
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Kim Yi-Soo
Lee Sung-Joong
Choi Jin-Young
Kim Yun-Hi
Desta Kebede Taye
Piao Zhe
Choi Su-Lim
Nam Sang-Jip
Kang Kyung-Yun
El Aty A. M. Abd
Shin Yong-Chul
Shin Sung-Chul
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Abstract
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β-N-acetylglucosamine (β-AG) is a monosaccharide distributed widely in living organisms with various pivotal roles. The presence of particulates and impurities can affect the safety and efficacy of a product for its intended duration of use. Thus, the current study was carried out to identify and quantify the potentially-harmful process related impurities; namely α-N,6-diacetylglucosamine (α-DAG) and α-N-acetylglucosamine (α-AG), derived from the chemical and enzymatic synthesis of β-AG. The impurities were characterized using a high resolution mass spectrometry, a nuclear magnetic resonance spectroscopy, and liquid chromatography-tandem mass spectrometry (LC/MS/MS). The developed method showed a good linearity (R2 ≥ 0.998), satisfactory precision (≤6.1 % relative standard deviation), intra- and inter-day accuracy (88.20?97.50 %), extraction recovery (89.30?110.50 %), matrix effect (89.70?105.20 %), and stability (92.70?101.60 %). The method was successfully applied to determine the level of α-DAG that was 3.04 and 0.07 % of the total β-AG, following chemical and enzymatic methods, respectively. It can be concluded that the enzymatic rather than the chemical method is more efficient for the synthesis of β-AG. Characterization of impurities heeds the signal for acquiring and evaluating data that establishes biological safety.
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KEYWORD
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β-N-acetylglucosamine, Process-related impurity, Tandem mass spectrometry, Chitin, Nuclear magnetic resonance
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