Institute for Control of Chinese Traditional Medicine and Ethnic Medicine, National Institutes for Food and Drug Control, Beijing, 100050, China; State Key Laboratory of Bioactive Substance and Function of Natural Medicines, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing, 100050, China.
Institute for Control of Chinese Traditional Medicine and Ethnic Medicine, National Institutes for Food and Drug Control, Beijing, 100050, China.
J Pharm Biomed Anal. 2019 Aug 5;172:149-166. doi: 10.1016/j.jpba.2019.03.049. Epub 2019 Mar 25.
Dianthrone derivatives are minor constituents of Polygonum multiflorum Thunb. (PM). These derivatives are potential hepatotoxic components in PM. Fraction D contains many dianthrone derivatives and was successfully enriched using an efficient three-step approach. An effective and reliable high-performance liquid chromatography (HPLC) technique coupled with ultraviolet detection (UV) and a linear ion trap FT-ICR hybrid mass spectrometry (HPLC-UV/LTQ-FT-ICR-MS) method were successfully developed to separate and identify the dianthrones of the fraction D. The characteristic diagnostic fragment ions and characteristic fragmentation pathway of the seven dianthrone standards, namely, Polygonumnolide B1 (S1), Polygonumnolide C3 (S2), Polygonumnolide C2 (S3), Polygonumnolide E (S4), Polygonumnolide A1 (S5), Polygonumnolide A2 (S6) and cis-emodin dianthrones (S7), were compared with unknown compounds in fraction D, and 45 dianthrone derivatives were characterized or tentatively identified. Of these derivatives, 32 new dianthrone derivatives were tentatively characterized in PM. Therefore, LTQ-FT-ICR-MS combined with a selective enrichment method provided a powerful means for analyzing dianthrone derivatives. This study provides a meaningful basis for correcting some mistakes in previous studies, as well as further quality control and pharmacological and toxicological research.
二蒽酮衍生物是何首乌（PM）的次要成分。这些衍生物是 PM 中潜在的肝毒性成分。馏分 D 含有许多二蒽酮衍生物，通过一种高效的三步方法成功得到了富集。成功开发了一种有效的、可靠的高效液相色谱（HPLC）技术，与紫外检测（UV）和线性离子阱傅里叶变换离子回旋共振混合质谱（HPLC-UV/LTQ-FT-ICR-MS）相结合，用于分离和鉴定馏分 D 的二蒽酮。七种二蒽酮标准品，即 Polygonumnolide B1（S1）、Polygonumnolide C3（S2）、Polygonumnolide C2（S3）、Polygonumnolide E（S4）、Polygonumnolide A1（S5）、Polygonumnolide A2（S6）和大黄素二蒽酮（S7）的特征诊断碎片离子和特征裂解途径，与馏分 D 中的未知化合物进行了比较，鉴定或初步鉴定了 45 种二蒽酮衍生物。这些衍生物中，32 种新的二蒽酮衍生物在 PM 中被初步鉴定。因此，LTQ-FT-ICR-MS 结合选择性富集方法为分析二蒽酮衍生物提供了有力的手段。本研究为纠正以往研究中的一些错误提供了有意义的依据，也为进一步的质量控制和药理毒理研究提供了依据。
