采用选择性带宽异核单量子相关谱（bs-qHSQC）对库拉索芦荟（Aloe barbadensis）和好望角芦荟（Aloe ferox）进行质量控制。

Quality control of Aloe vera (Aloe barbadensis) and Aloe ferox using band-selective quantitative heteronuclear single quantum correlation spectroscopy (bs-qHSQC).

机构信息

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.

出版信息

Talanta. 2019 Dec 1;205:120109. doi: 10.1016/j.talanta.2019.07.004. Epub 2019 Jul 2.

DOI:10.1016/j.talanta.2019.07.004

PMID:31450436

Abstract

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.

摘要

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。