多杀菌素潜在杂质的分离、鉴定与特性研究及其杀虫活性评价。
Isolation, identification, and characterization of potential impurities of doramectin and evaluation of their insecticidal activity.
机构信息
Department of Chemical and Chemical Engineering, Hefei Normal University, Hefei, 230601, People's Republic of China.
Chengdu Institute of Biology, Chinese Academy of Sciences, Chengdu, 610041, People's Republic of China; University of Chinese Academy of Sciences, Beijing 100049, People's Republic of China.
出版信息
J Pharm Biomed Anal. 2020 Nov 30;191:113600. doi: 10.1016/j.jpba.2020.113600. Epub 2020 Sep 9.
Seven impurities were detected in doramectin bulk drug by HPLC analysis. These impurities were named as Imp-I, Imp-II, Imp-III, Imp-IV, Imp-V, Imp-VI, and Imp-VII. All impurities were isolated from doramectin bulk drug by means of preparative HPLC. Among impurities, Imp-IV and Imp-V were unknown and have not been reported previously. Based on the complete spectral analysis, including 1D (H, C, H-D, DEPT 90 and 135), 2D (COSY, HSQC, HMBC, and NOESY) NMR, IR, and ESI-HRMS, the structure of Imp-IV and Imp-V were elucidated. Imp-IV was found to be a furan ring-opening product, while Imp-V lacked a methyl group at the C-14 in doramectin. Identification, isolation, structural characterization, probable formation mechanism, and insecticidal activity of impurities of doramectin were also discussed.
高效液相色谱法分析发现多拉菌素原料药中有 7 种杂质。这些杂质分别命名为 Imp-I、Imp-II、Imp-III、Imp-IV、Imp-V、Imp-VI 和 Imp-VII。所有杂质均通过制备高效液相色谱法从多拉菌素原料药中分离得到。其中杂质 Imp-IV 和 Imp-V 是未知的，以前没有报道过。基于包括 1D（H、C、H-D、DEPT 90 和 135）、2D（COSY、HSQC、HMBC 和 NOESY）NMR、IR 和 ESI-HRMS 在内的完整光谱分析，阐明了 Imp-IV 和 Imp-V 的结构。发现 Imp-IV 是呋喃环开裂产物，而 Imp-V 缺少多拉菌素 C-14 位上的甲基。还讨论了多拉菌素杂质的鉴定、分离、结构表征、可能的形成机制和杀虫活性。
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