羟丙基甲基纤维素乙酰琥珀酸酯药用辅料的校正固态13C核磁共振峰分配和侧基定量

IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY
Zhaoxi Zheng, Yongchao Su, Klaus Schmidt-Rohr
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引用次数: 0

摘要

羟丙基甲基纤维素乙酰琥珀酸酯(HPMCAS)是一种广泛应用的药用辅料,详细了解其可调结构对制剂设计具有重要意义。最近报道的HPMCAS固态13C NMR光谱中的几个峰分配已经在这里使用定量光谱中的峰积分、光谱编辑、基于溶液NMR的经验化学位移预测以及类似于去卷积的全谱模拟进行了校正。与纤维素不同,84处的强峰值 ppm必须分配给C2和C3甲基醚而不是纤维素的常规C4。在<;65 ppm到OCH位点,包括纤维素的C5,不能得到证实。CH2光谱编辑显示两个解析的OCH2带,一个来自C6的O-CH2醚的更强的带,在>;69 ppm和一个较小的来自其酯和可能残留的CH2-OH基团,接近63 ppm。乙酰基、琥珀酰基和氧丙基取代基的解析信号的强强度表明>;HPMCAS中85%的OH基团。对三种不同级别HPMCAS的副组浓度进行了定量。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

Corrected solid-state 13C nuclear magnetic resonance peak assignment and side-group quantification of hydroxypropyl methylcellulose acetyl succinate pharmaceutical excipients

Corrected solid-state 13C nuclear magnetic resonance peak assignment and side-group quantification of hydroxypropyl methylcellulose acetyl succinate pharmaceutical excipients

Hydroxypropyl methylcellulose acetyl succinate (HPMCAS) is widely used as a pharmaceutical excipient, making a detailed understanding of its tunable structure important for formulation design. Several recently reported peak assignments in the solid-state 13C NMR spectrum of HPMCAS have been corrected here using peak integrals in quantitative spectra, spectral editing, empirical chemical-shift predictions based on solution NMR, and full spectrum simulation analogous to deconvolution. Unlike in cellulose, the strong peak at 84 ppm must be assigned to C2 and C3 methyl ethers, instead of regular C4 of cellulose. The proposed assignment of signals at <65 ppm to OCH sites, including C5 of cellulose, could not be confirmed. CH2 spectral editing showed two resolved OCH2 bands, a more intense one from O-CH2 ethers of C6 at >69 ppm and a smaller one from its esters and possibly residual CH2-OH groups, near 63 ppm. The strong intensities of resolved signals of acetyl, succinoyl, and oxypropyl substituents indicated the substitution of >85% of the OH groups in HPMCAS. The side-group concentrations in three different grades of HPMCAS were quantified.

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来源期刊
CiteScore
4.70
自引率
10.00%
发文量
99
审稿时长
1 months
期刊介绍: MRC is devoted to the rapid publication of papers which are concerned with the development of magnetic resonance techniques, or in which the application of such techniques plays a pivotal part. Contributions from scientists working in all areas of NMR, ESR and NQR are invited, and papers describing applications in all branches of chemistry, structural biology and materials chemistry are published. The journal is of particular interest not only to scientists working in academic research, but also those working in commercial organisations who need to keep up-to-date with the latest practical applications of magnetic resonance techniques.
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