Quantum mechanical NMR full spin analysis in pharmaceutical identity testing and quality control.
Quantum mechanical NMR full spin analysis in pharmaceutical identity testing and quality control.
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DOI：
10.1016/j.jpba.2020.113601
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发表时间：
2021-01-05
影响因子：
3.4
通讯作者：
Pauli GF
中科院分区：
文献类型：
--
作者：
Achanta PS;Jaki BU;McAlpine JB;Friesen JB;Niemitz M;Chen SN;Pauli GF
与药品质量有关的问题正在以惊人的速度出现。药品质量涉及活性药物成分（API）和成品制剂/处方。最近，关于市售药物制剂中有害杂质的报告数量显著增加。杂质的范围从溶剂、反应物、掺杂物和催化剂到合成副产物。商业制剂中的质量问题也可能由于保质期稳定性而出现。此外，还报告了一些假药和劣药案件。目前使用的大多数技术充其量只能检测杂质，但不能识别它们，除非它们是已知的，并且可以与标准品进行比较。另一方面，1H NMR光谱检测所有含氢物质，通常提供信息以部分或甚至完全阐明结构，并且通过其绝对定量能力甚至可以间接检测无氢物质的存在。产生1H NMR信号作为给定分子的特征表示的结构性质是化学位移（δ，ppm）和耦合常数（J，Hz）。沿着线宽（ω1/2，Hz），这些参数通过量子力学（QM）原理与分子和NMR实验条件绑定。这意味着可以精确计算API的1H NMR谱，并与实验数据进行比较。这篇综述解释了1H NMR光谱与全自旋分析如何通过改善结构去复制和实现API及其污染物的同时定量来促进药物的质量控制。
Issues related to pharmaceutical quality are arising at an alarming rate. Pharmaceutical quality concerns both the Active Pharmaceutical Ingredients (APIs) and the Finished Drug Product/ Formulation. Recently, there has been a significant increase in the number of reports of harmful impurities in marketed drug formulations. Impurities range from solvents, reactants, adulterants, and catalysts to synthetic byproducts. Quality concerns in commercial preparations may also arise due to shelf life stability. Furthermore, a number of falsified and substandard drug cases have been reported. Most of the techniques which are currently in place can, at best, detect the impurities, but cannot identify them unless they are already known and can be compared to a standard. On the other hand, 1H NMR spectroscopy detects all the hydrogen containing species, typically provides information to elucidate structures partially or even completely, and through its absolute quantitative capabilities even can detect the presence hydrogen-free species indirectly. The structural properties that produce 1H NMR signals as characteristic representations of a given molecule are the chemical shifts (δ in ppm) and coupling constants (J in Hz). Along with the line widths (ω1/2 in Hz), these parameters are bound to both the molecule and the NMR experimental conditions by the quantum mechanical (QM) principles. This means that the 1H NMR spectra of APIs can be precisely calculated and compared to the experimental data. This review explains how 1H NMR spectroscopy coupled with Full Spin Analysis can contribute towards the quality control of pharmaceuticals by improving structural dereplication and achieving simultaneous quantification of both APIs and their contaminants.
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影响因子：
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