Department of Pharmaceutical and Medicinal Chemistry, Institute of Pharmacy, Kiel University, Gutenbergstraße 76, 24118, Kiel, Germany.
Department of Pharmaceutical Biology, Institute of Pharmacy, Kiel University, Gutenbergstraße 76, 24118, Kiel, Germany; Department of Chemistry 'Hugo Schiff', University of Florence, Via della Lastruccia 3-13, Sesto Fiorentino, 50019, Firenze, Italy.
Talanta. 2019 Dec 1;205:120109. doi: 10.1016/j.talanta.2019.07.004. Epub 2019 Jul 2.
In the present study, band-selective quantitative heteronuclear single quantum correlation spectroscopy (bs-qHSQC) was applied for the quality control of the two Aloe species present in the European Pharmacopeia. After development and validation of a complete spectral range (csr-) qHSQC assay, a specific pulse program with selective excitation was applied and the measuring time was reduced from 135 to 32 min, while maintaining the same resolution. This bs-qHSQC method (method I) showed slightly higher RSD values compared to the csr-qHSQC method (maximum RSD of 2.80%), but better recovery rates in comparison to the assay of the Pharmacopeia (97.3% for Aloe vera and 96.6% for Aloe ferox). Apart from quantifying the total anthranoid content, the method moreover allows the quantitation of aloin among other aloin derivatives, such as 7-hydroxyaloin, as well as the differentiation of the two investigated species. Additionally, a second bs-qHSQC method (method II) for the fast (4 min) determination of the aloin A/B ratio was developed and compared to C qNMR measurements. Showing the same results in much less analysis time, the latter approach contributes to a general problem in natural product chemistry, the co-occurrence of structurally similar compounds and their analysis in complex matrices, e.g. plant extracts.
在本研究中，带选择性定量异核单量子相关谱（bs-qHSQC）被应用于控制欧洲药典中两种芦荟物种的质量。在开发和验证完整谱范围（csr-）qHSQC 分析方法后，应用了具有选择性激发的特定脉冲程序，测量时间从 135 分钟缩短至 32 分钟，同时保持相同的分辨率。与 csr-qHSQC 方法（方法 I）相比，这种 bs-qHSQC 方法（方法 I）的 RSD 值略高（最大 RSD 为 2.80%），但与药典的测定相比，回收率更好（97.3%为库拉索芦荟和 96.6%为好望角芦荟）。除了定量测定总蒽醌含量外，该方法还可以定量测定芦荟苷以及其他芦荟苷衍生物，如 7-羟基芦荟苷，并且可以区分两种被研究的物种。此外，还开发了第二种 bs-qHSQC 方法（方法 II），用于快速（4 分钟）测定芦荟苷 A/B 比，并与 C qNMR 测量进行比较。由于分析时间大大缩短，该方法的结果相同，它有助于解决天然产物化学中的一个普遍问题，即结构相似的化合物的共同存在及其在复杂基质（如植物提取物）中的分析。
