Determination of scutellarin in breviscapine preparations using quantitative proton nuclear magnetic resonance spectroscopy.
Determination of scutellarin in breviscapine preparations using quantitative proton nuclear magnetic resonance spectroscopy.
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DOI：
10.1016/j.jfda.2015.12.004
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发表时间：
2016-04
影响因子：
3.6
通讯作者：
Wang, Yuefei
中科院分区：
文献类型：
--
作者：
Jiang, Zhenzuo;Yang, Jing;Jiao, Yujiao;Li, Wayne;Chai, Xin;Zhang, Lei;Jiang, Miaomiao;Wang, Yuefei
关键词：
本研究的目的是发展质子信号的选择标准，用于使用定量核磁共振（qNMR）测定灯盏乙素，这是治疗脑血管疾病的灯盏花素制剂中的主要生物活性化合物。选择3-（三甲基硅基）丙酸-2，2，3，3-d4酸钠盐的甲基单线态信号作为定量的内标。通过使用不同的质子信号来确定灯盏乙素的摩尔浓度。为了获得用于定量的最佳质子信号，根据两个选择标准研究了质子信号的不同组合：qNMR方法的回收率和与超高效液相色谱法获得的定量结果的比较。结果表明，H-2′和H-6′在δ 7.88处的化学位移是测定不同厂家、不同批号、不同剂型灯盏花素制剂中灯盏乙素含量的最佳信号，具有良好的线性范围、精密度和回收率。采用系统聚类分析对测定结果进行评价。结果表明，本工作建立的质子信号选择标准是可靠的灯盏花素制剂中灯盏乙素的qNMR研究。
The objective of the present study was to develop the selection criteria of proton signals for the determination of scutellarin using quantitative nuclear magnetic resonance (qNMR), which is the main bioactive compound in breviscapine preparations for the treatment of cerebrovascular disease. The methyl singlet signal of 3-(trimethylsilyl)propionic-2,2,3,3-d4 acid sodium salt was selected as the internal standard for quantification. The molar concentration of scutellarin was determined by employing different proton signals. To obtain optimum proton signals for the quantification, different combinations of proton signals were investigated according to two selection criteria: the recovery rate of qNMR method and quantitative results compared with those obtained with ultra-performance liquid chromatography. As a result, the chemical shift of H-2′ and H-6′ at δ 7.88 was demonstrated as the most suitable signal with excellent linearity range, precision, and recovery for determining scutellarin in breviscapine preparations from different manufacturers, batch numbers, and dosage forms. Hierarchical cluster analysis was employed to evaluate the determination results. The results demonstrated that the selection criteria of proton signals established in this work were reliable for the qNMR study of scutellarin in breviscapine preparations.
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