Miles Christopher O, Wilkins Alistair L, Jensen Dwayne J, Cooney Janine M, Quilliam Michael A, Aasen John, MacKenzie A Lincoln
National Veterinary Institute, PB 8156 Dep., 0033 Oslo, Norway.
Chem Res Toxicol. 2004 Nov;17(11):1414-22. doi: 10.1021/tx049832r.
41a-homoyessotoxin (1), a new analogue of yessotoxin (7), was isolated from extracts of Protoceratium reticulatum grown in culture. In addition, 9-methyl-41a-homoyessotoxin (2) and a nor-ring A-yessotoxin (3) were identified as the major components of a mixed fraction. The structural information was initially obtained from LC-UV and LC-MS3 chromatograms, with subsequent definitive structure determination by NMR, LC-MS/MS, and high-resolution MS. Full 1H and indirectly detected 13C NMR assignments for all but two carbon atoms were obtained from ca. 100 microg of 1. Full 1H NMR assignments for 2 and 3 and identification of three new heptanor-41-oxo-analogues of 3 (4-6) during LC-MS3 analysis of a fraction containing 1-3 and 7 are also reported.
41a-高叶软海绵毒素（1）是从培养的网状原角藻提取物中分离得到的一种新的叶软海绵毒素（7）类似物。此外，9-甲基-41a-高叶软海绵毒素（2）和去环A-叶软海绵毒素（3）被鉴定为一个混合组分的主要成分。结构信息最初通过液相色谱-紫外和液相色谱-串联质谱3色谱图获得，随后通过核磁共振、液相色谱-串联质谱/质谱和高分辨质谱进行最终的结构确定。从约100微克的1中获得了除两个碳原子外所有碳原子的完整氢谱和间接检测的碳谱归属。还报道了2和3的完整氢谱归属，以及在对含有1 - 3和7的一个组分进行液相色谱-串联质谱3分析过程中鉴定出3的三种新的庚去甲-41-氧代类似物（4 - 6）。
